GIFT  OF 
TU  Craif  Western  Sar 


METHODS  OF  ANALYSIS 

AND  LABORATORY 

CONTROL 

OF  THE 

GREAT  WESTERN  SUGAR 
COMPANY 


BY  THE 

CHEMICAL  DEPARTMENT 
OF  THE  GREAT  WESTERN  SUGAR  COMPANY 


FIRST    EDITION 


DENVER 

THE  GREAT  WESTERN  SUGAR  COMPANY 
1920 


*    . 
.    . 


- 


COPYRIGHT,  1920 

BY 
HE  GREAT  WESTERN  SUGAR  COMPANY 


PRINTED   BY 


PREFACE 

This  book  is  an  outgrowth  of  a  20-page  pamphlet,  "Methods 
of  Analysis  for  Beet  Sugar  Factories,"  published  in  1903,  and 
reissued  in  revised  form  in  1908.  With  the  development  of  a 
highly  specialized  system  of  chemical  control,  the  need  for  a  more 
up  to  date  and  comprehensive  treatise  has  been  increasingly  felt. 
The  present  book  has  accordingly  been  prepared  as  a  handbook 
and  reference  book  for  the  laboratories  of  the  Great  Western  Sugar 
Company. 

It  has  seemed  desirable  to  include  not  only  directions  for  the 
process  control,  but  also  methods  for  the  analysis  of  raw  materials 
and  for  such  other  analyses  as  the  chemist  in  our  organization  is 
commonly  called  on  to  make.  This  has  resulted  in  the  expansion 
of  the  book  to  a  considerable  size,  but  at  the  same  time  an  effort 
has  been  made  to  employ  a  certain  conciseness  of  treatment  and 
style.  Hence  very  little  explanation  is  ordinarily  given  of  the 
reasons  for  various  steps  or  procedures,  except  where  the  reason 
is  likely  to  be  obscure  or  where  it  is  desired  to  emphasize  the  im- 
portance of  the  matter  in  the  reader's  mind.  It  is  expected  that 
the  chemist  will  be  able  readily  to  figure  out  such  things  for  him- 
self, and  to  profit  if  any  mental  exercise  is  involved.  For  the  sake 
of  keeping  the  book  within  reasonable  bounds,  directions  for  purely 
numerical  or  statistical  calculations  have  also,  with  a  few  excep- 
tions, been  purposely  omitted. 

A  great  number  of  chemists  of  this  company,  past  and  pres- 
ent, too  numerous  to  mention,  are  responsible  for  the  development 
of  our  methods  of  analysis  and  laboratory  control  to  their  present 
status.  The  writer's  thanks  are  due  in  particular  to  Mr.  P.  Roller 
for  assistance  in  preparing  a  considerable  portion  of  the  manu- 
script and  for  having  read  over  the  text  in  its  entirety. 

The  following  books  have  been  consulted  and  found  especially 
helpful:  Browne's  "Handbook  of  Sugar  Analysis,"  Hillebrand's 

iii 

468640 


iv  •  PREFACE 

"The  Analysis  of  Silicate  and  Carbonate  Rocks"  (Bulletin  700  of 
the  U.  S.  Geological  Survey),  Scott's  "Standard  Methods  of  Chemi- 
cal Analysis,"  the  "Methods  of  Analysis"  of  the  Association  of 
Official  Agricultural  Chemists,  and  Circular  44,  "  Polarimetry, " 
and  numerous  other  publications  of  the  Bureau  of  Standards.  For 
the  methods  for  the  analysis  of  diatomaceous  earth  we  are  indebted 
to  Messrs.  S.  C.  Meredith  and  P.  B.  Caster,  of  the  Western  Sugar 
Refining  Company. 

The  writer  will  especially  welcome  criticisms  from  any  source 
which  will  assist  him  in  correcting  errors  or  making  improvements 
in  a  future  edition. 

S.  J.  OSBORN 

General  Chemist, 

The  Great  Western  Sugar  Company. 

Denver,  Colorado,  July  29,  1920. 


CONTENTS 

Chapter  Page 

I.     GENERAL  METHODS    1 

II.     REGULAR  FACTORY  CONTROL 16 

III.  SULPHATE  CONTROL   42 

IV.  STEFFEN  PROCESS  CONTROL 47 

V.     PULP   DRYER   CONTROL 62 

VI.     PULP  SILO  CONTROL 691 

VII.     BOILER  HOUSE  CONTROL 72 

VIII.     POTASH  CONTROL   (BEET  CAMPAIGN) 80 

IX.     POTASH   CONTROL    (POTASH    CAMPAIGN) 82( 

X.     CRUDE  POTASH   90 

XI.     MOLASSES     100 

XII.     BEET  LABORATORY   TESTS 102 

XIII.  ASH  ANALYSIS  OF  SUGAR  FACTORY  PRODUCTS 107 

XIV.  SCALES  AND  DEPOSITS 115 

XV.     COAL  AND  COKE 126) 

XVI.     LIMESTONE     133 

XVII.     WATER 139 

XVIII.     DIATOMACEOUS  EARTH    (KIESELGUHR) 147 

XIX.     SULPHUR     : 149 

XX.     FOODS  AND  FEEDING   STUFFS 151 

XXI.     COTTON    SEED  CAKE 157 

XXII.     SOIL    160 

XXIII.  APPARATUS    168 

XXIV.  STANDARDIZATION  AND  VERIFICATION  OF  APPARATUS .  179 
XXV.     REAGENTS     188 

XXVI.  MISCELLANEOUS                                                                               ...198 


VI  CONTENTS 

Chapter  Page 

XXVII.     TABLES 

1.  Brix,  Baume,  and  Specific  Gravity  of  Sugar  Solutions.  .201 

2.  Factors  for  Calculation  of  Apparent  Purity 214 

3.  Temperature  Corrections  for  Brix  Hydrometers — Stand- 

ard Temperature  20  °   C 215 

3-A.     Temperature  Corrections  for  Brix  Hydrometers — Stand- 
ard Temperature  20°  C.     (Condensed  Table) 216 

4.  Temperature   Corrections  for  the  Abbe   Sugar  Refrac- 

tometer — Standard  Temperature  20°   C 216 

5.  Approximate  Amounts  of  Basic  Lead  Acetate  Solution 

(55°  Brix)  for  Various  Products 217 

6.  Polarization  Table— 200  mm  Tube,  1/10  Dilution.     (For 

Pulp  and  Pulp  Water) 218 

7.  Polarization  Table— 400  mm  Tube,  1/10  Dilution.     (For 

Sewer  Water)    218 

8.  Polarization  Table— 400  mm  Tube,  Read  Direct.     (For 

Condensed  Waters)    219 

9.  Steffen  Polarization  Table 220 

10.  Invert     Sugar    in     Thick    Juices,     Syrups,     and     Solid 

Products     221 

11.  Invert  Sugar  in  Thin  Juices 223 

12.  Cupric   Oxide   Table  for   Obtaining  the  Percentage   of 

Invert  Sugar  (10  grams  of  material) 223 

13.  Cupric   Oxide   Table   for   Obtaining  the   Percentage   of 

Invert  Sugar  (5  grams  of  material) 223 

14.  CaO  by  Soap  Solution  in  Thin  Juices 224 

15.  CaO   by    Soap    Solution    in   Thick   Juices,    Massecuite, 

Molasses,   etc 226 

16.  Table    for    Use    in    Dry    Substance    Determinations    on 

Pulp  Sold 228 

17.  B.  T.  U.  Lost  in  Dry  Flue  Gas  per  pound  of  Coal  Con- 

taining 57%  Carbon 229 

18.  "Moisture  Factor"  for  Computing  Loss  of  Heat  in  Flue 

Gas  due  to  Moisture 241 

18-A.     "Temperature  Factor"  for  Computing  Loss  of  Heat  in 

Flue  Gas  due  to  Moisture 242 

19.  CaO  in  Milk  of  Lime  of  Various  Densities 243 

20.  Equivalents  of  Normal  Solutions 244 

21.  Percentage  of  Available  Granulated  on  Dry  Substance 

of  Sugar  Solutions — Molasses  Purity  of  60 245 

22.  Percentage  of  Available  Granulated  on  Total  Sugar  of 

Sugar  Solutions — Molasses  Purity  of  60 246 

23.  Standard  Beet  Extraction 247 

24.  Standard  Steffen  Extraction 251 

25.  Specific  Gravity  of  Various  Materials 251 

26.  International  Atomic  Weights,  1920 252 

INDEX    .  253 


I.  GENERAL  METHODS 
1.  DEGREES  BRIX 

The  Brix  scale  represents  the  percentage  of  sugar  in  a  pure 
sugar  solution.  The  reading  of  a  Brix  hydrometer  in  a  solution  at 
the  standard  temperature  (20°  C.)  is  known  as  the  "degrees  Brix," 
or  simply  the  "Brix,"  which  is  employed  as  an  approximate  meas- 
ure of  the  percentage  of  dry  substance. 

(a)     DIRECT  METHOD 

Determine  the  density  of  all  solutions  up  to  75°  Brix  as  fol- 
lows: Transfer  the  solution  to  a  suitable  glass  cylinder  (hydro- 
meter jar),  and,  if  necessary,  immerse  in  a  cooling  bath  to  reduce 
the  temperature  to  approximately  20°.  If  air  bubbles  are  present, 
remove  them  by  the  action  of  a  vacuum.  Mix  the  solution  in  the 
cylinder  to  equalize  the  temperature  and  immerse  a  clean,  dry 
hydrometer  about  one-quarter  of  an  inch  below  the  point  where  it 
floats  naturally  and  then  allow  it  to  assume  its  normal  position. 
Read  the  scale  by  bringing  the  eye  upon  a  level  with  the  surface 
of  the  solution  so  that  the  latter  appears  as  a  straight  line  and 
not  an  ellipse,  and  note  where  the  border  line  forming  the  bottom 
of  the  meniscus  intersects  the  scale.  Dark  or  opaque  solutions 
may  have  to  be  read  from  above,  by  estimating  the  distance  of  the 
level  of  the  solution  below  the  top  of  the  meniscus.  When  the 
reading  is  taken,  the  liquid  and  hydrometer  must  be  free  from  air 
bubbles  and  at  rest,  and  the  hydrometer  must  not  be  in  contact  witli 
the  bottom  or  walls  of  the  cylinder. 

Take  the  temperature  of  the  solution  with  a  thermometer; 
if  it  is  not  exactly  20°,  apply  the  correction  indicated  in  Table 
3  or  3-A.  Hydrometer  readings  should  not  be  made  below  15° 
or  above  25°. 

To  insure  strict  accuracy,  the  cylinder  should  be  filled  so  full 
that  the  insertion  of  the  hydrometer  causes  the  liquid  to  overflow. 


2  METHODS  OP  ANALYSIS 

This  minimizes  the  effect  on  the  reading  of  the  formation  of  sur- 
face films  of  impurities. 

(b)     DOUBLE  DILUTION  METHOD 

In  the  case  of  molasses,  massecuite,  etc.,  weigh  out  400  grams 
in  a  copper  beaker,  add  about  350  grams  of  hot  water,  and  stir 
with  a  glass  rod  until  completely  dissolved.  Cool  to  approximately 
20°,  remove  and  rinse  the  rod,  make  up  to  800  grams  with  water, 
and  mix  well.  Pour  into  a  glass  cylinder,  rinsing  it  first  with  a 
little  of  the  solution  if  the  cylinder  is  wet,  and  obtain  the  Brix 
reading  as  under  (a).  Apply  the  temperature  correction,  if  neces- 
sary, and  then  multiply  by  2.  Other  weights  may  be  used  if  the 
final  dilution  is  in  the  same  ratio. 

See  under  "4.  Apparent  Purity  Determination"  regarding 
the  quality  of  the  water  used  for  dilution. 

2.     DRY  SUBSTANCE  AND  MOISTURE 

Special  directions  for  particular  products  will  be  found  under 
"Sugar,"  "Dried  Pulp,"  etc.  Where  this  determination  is  im- 
portant in  itself,  other  than  as  an  incidental  figure  for  obtaining 
the  true  purity,  etc.,  it  should  not  be  made  on  material  which  has 
been  placed  under  vacuum  for  any  great  length  of  time,  because  a 
considerable  increase  in  concentration  sometimes  occurs  under  this 
condition. 

(a)     BY  OVEN  DRYING 

( 1 )  Apparatus :     A  double-walled  drying  oven  containing  a 
glycerin  solution  in  the  jacket,  of  such  a  strength  that  a  tempera- 
ture of  100-105°  is  maintained  in  the  interior  of  the  oven.     The 
boiling  point  is  kept  constant  by  means  of  a  reflux  condenser.    See 
Chap.  XXIII,  7. 

Aluminum  dishes  2  in.  diameter  by  11/2  in-  high,  as  described 
in  Chap.  XXIII,  6,  provided  in  each  case  with  an  aluminum  cover 
and  a  glass  rod  of  such  a  length  that  it  will  not  interfere  with  the 
proper  position  of  the  cover. 

A  desiccator  containing  sulphuric  acid  as  the  dehydrating 
agent.  The  acid  should  be  renewed  as  soon  as  it  shows  any  sign  of 
discoloration  or  loss  of  absorptive  power.  Renew  the  acid  at  least 
once  a  week  when  the  desiccator  is  in  constant  use. 

(2)  Reagents:     Sea  sand   prepared   as   described   in   Chap. 
XXV,  17. 


I.      GENERAL  METHODS  3 

(3)  Method:  Place  25-30  grams  of  sea  sand  in  an  aluminum 
dish  and  dry  it,  together  with  the  cover  and  glass  rod,  in  an  oven 
at  100-105°  C.  for  at  least  one  hour.  Remove  from  the  oven,  put 
on  the  cover,  and  cool  in  a  desiccator. 

Weigh  out,  in  'the  covered  aluminum  dish,  an  amount  of  the 
material  under  examination  which  is  equivalent  to  approximately 
one  gram  of  dry  substance.  Warm  the  dish  on  top  of  the  drying 
oven,  remove  the  cover,  and  mix  the  contents  well.  Warm  again, 
add  1  ml  of  *hot  water  and  stir  until  a  perfectly  homogeneous 
mixture  is  obtained.  Dry  at  100-105°  C.  for  5-6  hours,  replace 
the  cover,  cool  in  the  desiccator,  and  weigh.  Repeat  the  drying 
for  one  hour  periods  until  the  loss  in  weight  in  any  period  is  less 
than  0.1%.  Keep  the  thermometers  in  the  desiccator  and  balance 
case,  and  do  not  make  the  weighings  until  the  difference  in  tem- 
perature is  2  degrees  or  less. 

Make  all  determinations  in  duplicate.  The  duplicates  should 
ordinarily  check  within  0.1% ;  if  they  differ  by  more  than  0.2% 
repeat  the  determination. 

Sugar,  dried  pulp,  and  filter  press  cakes  are  dried  directly 
without  the  use  of  sand. 

(b)     BY  REFRACTOMETER 

The  Abbe  sugar  refractometer  uses  the  refractive  index  as  a 
measure  of  the  percentage  of  dry  substance,  and  in  the  case  of  or- 
dinary sugar  factory  products  gives  results  which  are  close  to  those 
found  by  oven  drying. 

Use  the  original  material  in  the  case  of  juices,  syrups,  and 
molasses,  and  " double  diluted"  material  in  the  case  of  sugar  and 
massecuite.  Place  1  or  2  drops  on  one  of  the  prisms,  close  quickly, 
mid  circulate  water  at  20°  through  the  instrument.  Read  directly 
from  the  scale  the  percentage  of  dry  substance.  Multiply  the 
reading  by  two  if  "double  diluted"  material  has  been  used.  If 
the  reading  is  not  made  at  exactly  20°,  apply  the  correction  indi- 
cated in  Table  4.  Check  the  zero  point  of  the  instrument  frequently 
with  distilled  water.  See  also  Chap.  XXIII,  16  and  XXIV,  8. 

3.     SUGAR 

The  polarization  (direct  polarization)  is  defined  as  the  per- 
centage of  sugar  indicated  by  the  polariscope. 


*Thin  solutions  do  not  require  the  addition  of  water. 


4  METHODS  OF  ANALYSIS 

In  the  absence  of  other  optically  active  bodies  the  polarization 
represents  the  true  percentage  of  sugar.  In  the  presence  of  an- 
other optically  active  substance,  such  as  raffinose,  the  method  of 
double  polarization  (before  and  after  inversion)  is  used  to.  deter- 
mine the  two  sugars  accurately.  The  percentage  of  sugar  obtained 
in  this  manner  is  known  as  the  " sugar  by  inversion." 

(a)     SUGAR  BY  DIRECT  POLARIZATION 

Weigh  out  26  grams  (or  a  *fraction  or  multiple  thereof,  de- 
pending on  the  nature  of  the  material)  in  a  counterpoised  nickel 
dish,  and  dissolve  in  a  small  amount  of  water.  Use  hot  water  if 
difficult  to  dissolve.  Rinse  into  a  100  ml  flask  and  add  sufficient 
basic  lead  acetate  solution  to  decolorize,  avoiding  any  great  excess. 
(See  Table  5.)  Where  the  amount  of  the  lead  precipitate  is  small, 
as  in  the  case  of  products  of  high  purity,  the  addition  of  a  few 
drops  of  alumina  cream  will  aid  in  securing  a  clear  filtrate.  Cool 
to  approximately  20°  if  necessary,  and  make  up  to  the  mark  with 
water,  using  one  or  two  drops  of  ether,  if  necessary,  to  break  the 
foam.  Shake  well  and  filter,  rejecting  the  first  portion  of  the  fil- 
trate and  returning  the  remainder  to  the  filter  until  it  is  perfectly 
clear.  Polarize  in  a  200  mm  tube,  first  rinsing  the  tube  two  or 
three  times  with  the  solution.  If  the  normal  weight,  100  ml  flask, 
and  200  mm  tube  have  been  used,  the  reading  gives  directly  the 
percentage  of  sugar.  If  the  weight,  volume,  or  length  of  tube 
differs  from  these  standards,  calculate  the  percentage  of  sugar 
proportionally. 

When  great  accuracy  is  required,  make  up  to  the  mark  with 
water  at  exactly  20°  and  polarize  in  a  jacketed  tube  at  the  same 
temperature.  For  ordinary  work  it  is  sufficiently  accurate  to  ap- 
proximate the  above  temperature  conditions. 

See  also  Chap.  XXIII,  13,  regarding  the  use  of  the  polariscope. 

(b)     SUGAR  BY  INVERSION 

(1)  Polarize  as  above. 

(2)  Weigh   out  13   grams  of  the   original   material    (or  26 
grams  of  the  double  diluted  solution)   in  a  counterpoised  nickel 
dish,  dissolve  in  a  small  amount  of  water,  and  rinse  into  a  thin 
walled  100  ml  Kohlrausch  flask,  marked  at  the  point  at  which  it 
holds  75  ml.     Add  from  a  pipette  10  ml  of  hydrochloric  acid 

*In  the  case  of  molasses  use  13  grams  of  the  original  molasses,  or  26 
grams  of  the  "double  diluted"  solution.  In  the  case  of  other  products  of 
higher  purity  use  ordinarily  26  gram?  of  the  original  material,  or  52  grams 
ot  the  "double  diluted"  splution, 


I.       GENERAL   METHODS  5 

C)f\O 

(D  -^-1.029^see  Chap.  XXV,  10),  make  up  immediately  to  the 
75  ml  mark  with  water,  and  mix  thoroughly.  Place  a  thermometer 
in  the  flask,  and  immerse  in  a  water  bath  at  70°  with  frequent 
•agitation.  The  solution  should  reach  a  temperature  of  67°  in  not 
more  than  five  minutes,  and  preferably  in  2 — 3  minutes. 
When  the  temperature  reaches  67°,  note  the  time,  and  maintain 
the  temperature  for  exactly  five  minutes  between  67  and  70°.  Shake 
the  flask  occasionally  with  a  rotary  motion  in  order  that  the  tem- 
perature may  be  uniform  throughout  the  solution.  Then  place  the 
riask  immediately  in  a  cold  water  bath  and  cool  as  rapidly  as  pos 
sible  to  20°.  Remove  the  thermometer,  rinsing  the  adhering  liquid 
into  the  flask,  and  make  up  to  the  100  ml  mark  with  water  at  ex- 
actly 20°. 

Next  add  2-4  grams  of  zinc  dust,  according  to  the  amount  of 
decolorization  required,  and  allow  to  stand  for  half  an  hour, 
shaking  at  frequent  intervals.  Filter  and  polarize  at  exactly  20° 
in  a  200  mm  jacketed  tube. 

In  making  the  polarization,  place  the  tube  in  the  trough  of 
the  polariscope  and  insert  a  thermometer  graduated  in  one-tenths 
of  one  degree,  allowing  the  bulb  to  rest  against  the  bottom  of  the 
inner  tube.  Circulate  the  cooling  water  at  20°  (or  at  19-20°,  but 
never  below  19°)  until  the  thermometer  indicates  that  the  20° 
point  has  been  reached,  then  remove  the  thermometer  and  take  a 
sufficient  number  of  readings  with  as  little  delay  as  possible.  If 
the  solution  is  cooled  in  this  manner,  the  temperature  will  not 
change  appreciably  during  the  time  that  the  readings  are  made. 
Do  not  handle  the  tube  during  the  final  adjustment  of  the  tem- 
perature. 

All  the  conditions  prescribed  must  be  rigidly  followed  to  ob- 
tain accurate  results.  The  total  volume  during  inversion  must 
be  approximately  75  ml;  the  hydrochloric  acid  must  be  measured 
accurately  and  be  of  the  proper  strength ;  the  conditions  regarding 
the  temperature  and  time  of  heating  must  be  observed;  and  the 
solution  in  the  polariscope  tube  must  be  cooled  in  the  manner  de- 
scribed in  order  that  the  reading  may  be  made  at  exactly  20° 
and  that  this  temperature  may  prevail  uniformly  throughout  the 
solution.  Means  should  be  provided  for  a  sufficient  supply  of  cool- 
ing water  at  constant  temperature. 

^Fultiply  the  reading  by  2,  since  the  half -normal  weight  has 
been  used. 


*Mix  constantly  until  the  solution  has  attained  a  temperature  of  67°. 


D  METHODS  OP  ANALYSIS 

(c)     FORMULAS 

^(1)  Raffinose  Formula  (For  the  determination,  of  sugar  in 
the  presence  of  raffinose)  :  This  formula  is  generally  used  in  beet 
sugar  work. 

Let  P  =  direct  polarization 

J  =  polarization  after  inversion  (expressed  as  a  posi- 

tive number) 

S  =  %  sugar  by  inversion 
R  =       raffinose 


.839 
AndR  =  .54X  (P—  -S) 

(2)     Clerget  Formula  (For  the  determination  of  sugar  in  the 
presence  of  invert  sugar)  :  This  formula  is  not  commonly  used  in 
beet  sugar  work,  but  is  given  here  for  the  sake  of  completeness  : 
Let  T  =  temperature  at  which  polarization  is  made 

ThcnS 


142.66  —  .5  T 
Or,  if  T  =  20 

100  (P  +  J) 
132.66 

4.     APPARENT  PURITY 

(a)  DEFINITION 

The  "purity"  (coefficient  of  purity)  of  a  juice,  syrup,  etc., 
is  the  percentage  of  sugar  in  the  total  solid  matter,  and  is  calcu- 
lated by  multiplying  the  percentage  of  sugar  by  100  and  dividing 
by  the  percentage  of  solids.  If  the  direct  polarization  is  used  to 
represent  the  percentage  of  sugar  and  the  degrees  Brix  to  repre- 
sent the  percentage  of  solids,  the  result  is  known  as  the  '  '  apparent  '  ' 
purity.  If  the  '  '  sugar  by  inversion  '  '  is  used  for  the  percentage  of 
sugar  and  the  actual  dry  substance  for  the  percentage  of  solids,  the 
figure  is  known  as  the  '  '  true  '  '  purity. 

(b)  DETERMINATION 

If  too  thick,  dilute  the  material  with  water  to  approximately 
23°  Brix  as  follows  :  Put  a  suitable  amount  of  hot  water  in  a  copper 
can  or  sample  bucket,  and  add  a  suitable  amount  of  the  juice  or 
syrup;  the  proportions  to  be  used  should  be  such  as  will  yield  a 
solution  of  the  required  density  and  will  be  learned  by  experience. 


I.      GENERAL,  METHODS  7 

Stir  vigorously  until  completely  dissolved  and  then  pour  the  solu- 
tion into  a  cylinder  (hydrometer  jar).  The  solution  prepared  in 
this  manner  should  have  a  density  of  not  less  than  21°  nor  more 
than  24°  Brix.  If,  after  cooling  as  described  below,  the  density 
is  found  to  be  a  little  too  high,  add  the  necessary  small  amount  of 
cold  water,  and  mix  thoroughly  by  inverting  the  cylinder  at  least 
half  a  dozen  times;  only  under  this  condition  is  it  permissible  to 
make  any  dilutions  in  cylinders  or  with  the  use  of  cold  water,  and 
care  should  be  taken  then  that  a  thorough  mixture  is  obtained. 

" Double  diluted"  solutions,  if  available,  may  be  used  in  place 
of  the  original  material,  but  the  dilution  should  be  made  by  mixing 
with  hot  water  as  described  above  and  not  in  a  cylinder.  It  may 
be  preferable,  however,  in  order  to  save  time,  to  prepare  a  sep- 
arate solution  for  the  apparent  purity  determination  from  the 
original  material. 

Cool  in  the  cylinder  under  vacuum  to  remove  air  bubbles,  and 
obtain  the  Brix  reading  as  described  in  section  1,  "Degrees  Brix," 
making  correction  for  temperature  if  necessary.  Measure  out  100 
ml  in  a  100-110  nil  flask,  rinsing  the  latter  first  with  a  small  portion 
<•!'  the  solution,  and  add  sufficient  basic  lead  acetate  solution  for 
decolorization,  but  avoid  any  great  excess.  (See  Table  5.)  Fill 
to  the  110  ml  mark  with  water,  using  1  or  2  drops  of  ether,  if 
necessary,  to  break  the  foam.  Shake  well  and  filter,  rejecting  the 
first  portion  of  the  filtrate  and  returning  the  remainder  to  the  filter 
until  it  is  perfectly  clear.  Polarize  in  a  200  mm  tube,  first  rinsing 
the  tube  two  or  three  times  with  the  solution. 

Multiply  the  polariscope  reading  by  the  factor  corresponding 
to  the  corrected  Brix,  as  found  in  Table  2,  to  obtain  the  apparent 
purity.  To  simplify  this  calculation,  *tables  have  been  prepared 
covering  a  range  of  8-25°  Brix,  in  which  the  purity  is  derived  di- 
rectly from  the  Brix  and  the  polariscope  reading. 

It'  may  sometimes  be  necessary  to  use  a  100  mm  tube  for  the 
polarization  of  molasses  and  dark  syrups;  this  should  be  avoided, 
however,  if  possible. 

(c)     QUALITY  OF  WATER  USED  FOR  DILUTION 

The  quality  of  water  used  for  dilution  must  be  closely  investi- 
gated and  watched.  Most  water  is  not  high  enough  in  solids  to  af- 
fect a  purity  determination,  but  some  factory  water  supplies  are 
unsuitable  even  for  this  purpose  and  in  such  cases  distilled  water 
should  IK*  used.  If  the  alkalinity  of  the  product  is  to  be  subse- 


*"Laboratory  Tables,"  The  Great  Western  Sugar  Company,  1917. 


8  METHODS  OF  ANALYSIS 

quently  determined,  only  neutral  water  should  be  employed  for 
dilution;  and,  if  the  soap  test  is  to  be  made,  distilled  water  of  a 
small  and  determined  soap  value  should  be  used. 

5.     TEUE  PURITY 

Obtain  the  percentage  of  sugar  by  inversion  as  described  in 
section  3,  "Sugar,"  and  the  percentage  of  dry  substance  by  oven 
drying  or  by  the  refractometer  as  in  section  2,  "Dry  Substance 
and  Moisture." 

Let  S  =  %  sugar  by  inversion 
D  =  %dry  substance 
P  =  true  purity 
100  S 


Then  P  = 


I) 


6.     INVERT  SUGAR 


(a)     IN  THICK  JUICES,  SYRUPS,  AND  SOLID  PRODUCTS 

Determine  the  amount  of  material  to  be  used  by  reference  to 
Table  10.  Weigh  out  the  number  of  grams  indicated,  dissolve  in 
hot  water  and  rinse%  into  a  200  ml  flask.  Cool  if  necessary,  and  add 
sufficient  neutral  lead  acetate  solution  for  clarification,  avoiding 
any  great  excess,  fill  to  the  mark  with  water,  shake  well,  and  filter. 
Measure  out  100  .ml  of  the  filtrate  in  a  100-110  ml  flask,  add 
enough  of  a  strong  sodium  carbonate  solution  to  precipitate  all  the 
excess  of  lead,  complete  the  volume  to  110  ml  with  water,  shake 
well,  and  filter.  Transfer  50  ml  of  the  filtrate  (representing  10 
grams  of  dry  substance  of  the  original  material),  measured  with  a 
pipette,  to  an  Erlenmeyer  flask  of  about  250  ml  capacity  containing 
50  nil  of  Fehling's  Solution,  i.  e.  25  ml  each  of  the  copper  sulphate 
and  Rochelle  salt  solutions.  Heat  the  flask  with  a  flame  so  regu- 
lated that  the  solution  begins  to  boil  in  at  least  3^-4  minutes; 
take  the  time  at  which  boiling  commences  as  the  point  at  which 
bubbles  begin  to  rise  not  only  in  the  middle,  but  also  at  the  sides 
of  the  flask.  Boil  for  exactly  2  minutes,  and  then  cool  by  adding 
100  ml  of  cold,  distilled  water.  Allow  to  stand  for  not  more  than 
2  minutes  to  let  the  precipitate  settle,  and  filter  at  once  through 
an  ashless  filter  paper.  Wash  with  hot  water,  distribute  the  pre- 
cipitate over  the  filter  as  evenly  as  possible  with  a  glass  rod,  and 
ignite  in  a  porcelain  crucible.  Or  use  an  alundum  crucible  for 


I.      GENERAL  METHODS  . 

both  the  filtration  and  the  ignition.  From  the  weight  of  cupric 
oxide  obtained  find  the  corresponding  percentage  of  invert  sugar  in 
Table  12. 

If  the  amount  of  cupric  oxide  is  beyond  the  limit  of  the  table, 
use  25  ml  of  the  second  filtrate  with  25  ml  of  water  and  50  ml  of 
Fehling's  solution,  carrying  out  the  determination  as  before,  and 
obtain  the  percentage  of  invert  sugar  from  Table  13. 

Note  that  the  percentage  found  is  based  on  100  parts  dry  sub- 
stance or  Brix,  and  not  on  the  original  material. 

If  the  cupric  oxide  weighed  is  in  excess  of  300  mg,  the  results 
cannot  be  relied  on  because  of  the  difficulty  of  oxidizing  all  the 
copper.  In  such  a  case  the  precipitate  may  be  collected  on  an  as- 
bestos filter  in  a  glass  filter  tube,  ignited  in  a  current  of  hydrogen 
and  weighed  as  metallic  copper;  or  the  copper  may  be  determined 
by  the  Low  volumetric  method  given  in  Chap.  XIV,  6. 

For  larger  percentages  of  invert  sugar  beyond  the  limit  of  the 
cupric  oxide  table  use  a  *modified  Soxhlet  volumetric  method. 

(b)     IN  THIN  JUICES 

Determine  the  amount  of  material  to  be  used  by  reference  to 
Table  11.  Weigh  out  the  number  of  grams  indicated,  rinse  into  a 
200  ml  flask,  and  proceed  as  in  (a).  The  final  50  ml  taken  for  treat- 
ment with  Fehling's  Solution  will  contain  5  grams  of  dry  sub- 
stance. Obtain  the  " Invert  per  100  Brix"  from  Table  13. 

7.     ASH 

(a)     SULPHATED  ASH 

Where  the  term  "ash"  is  employed  without  any  qualifying 
expression,  sulphated  ash  is  understood  to  be  meant. 

Use  2  grams  of  molasses  and  larger  amounts  of  products  con- 
taining less  ash.  Weigh  out  quickly  in  a  platinum  crucible,  or 
better  a  porcelain  evaporating  dish  of  about  35  ml  capacity,  making 
no  attempt  to  weigh  a  definite  amount.  Do  not  use  silica  ware. 
Place  on  a  tHillebrand  radiator,  add,  if  necessary,  enough  water 
to  reduce  to  the  consistency  of  thick  juice,  and  evaporate  until  the 
bubbles  start  to  puff  up  in  the  dish.  At  this  point  remove  the  dish, 
and  add  concentrated  sulphuric  acid  a  drop  at  a  time  around  the 
edge  of  the  dish  until  the  entire  mass  is  black  and  ceases  to  boil. 


*Browne's  "Handbook  of  Sugar  Analysis,"  p.  391. 
tChap.  XXIII,  15. 


10  METHODS  OF  ANALYSIS 

Replace  on  the  radiator,  drive  off  the  excess  of  sulphuric  acid, 
and  ignite  at  a  dull  red  heat  in  a  muffle  till  the  carbon  is  com- 
pletely consumed.  The  resulting  ash  should  be  white  or  nearly  so 
and  should  not  be  allowed  to  fuse.  After  cooling,  resulphate  the 
ash  with  3  or  4  drops  of  dilute  sulphuric  acid  (1:10),  heat  first 
on  the  radiator,  and  then  ignite  at  a  dull  red  heat  for  a  minute 
or  two  over  a  flame.  Cool  in  a  desiccator  and  weigh. 

Subtract  one-tenth  of  the  weight  of  the  ash  to  compensate 
for  the  conversion  of  other  salts  to  sulphates.  This  correction  is 
known  to  be  seriously  in  error  but  is  maintained  in  accordance  with 
general  practice. 

(b)     LIXIVIATED  ASH 

Weigh  out  the  same  amount  as  prescribed  under  "Sulphated 
Ash "  in  a  platinum  dish ;  the  use  of  either  porcelain  or  silica  ware 
is  inadmissible.  Heat  over  B  flame,  applying  it  around  the  outer 
edge  to  prevent  material  being  pushed  over  the  side  of  the  dish 
by  the  escape  of  steam  and  gases.  After  most  of  the  volatile  mat- 
ter has  passed  off  and  the  organic  matter  is  completely  carbonized, 
crush  the  mass  to  a  fairly  fine  powder  by  means  of  an  agate  pestle 
and  heat  again  at  a  dull  redness.  A  too  high  temperature  of  heat- 
ing, which  will  cause  some  of  the  salts  to  fuse  and  volatilize,  will 
usually  be  indicated  by  the  formation  of  white  spots  on  the  dish, 
which  are  more  easily  seen  on  the  addition  of  the  water.  Remove 
from  the  flame  when  the  carbon  ceases  to  glow,  cool,  add  20  ml  of 
water,  place  on  a  hot  plate  and  allow  to  simmer  for  about  fifteen 
or  twenty  minutes,  replacing  the  evaporated  portion  with  hpt  water 
previous  to  filtration.  Filter  through  an  ashless  filter  paper  into  a 
100  ml  beaker,  washing  all  of  the  carbon  possible  into  the  filter, 
wash  twice  with  hot  water,  and  evaporate  to  a  small  volume. 

Dry  the  platinum  dish  carefully  and  ignite  it  until  any  ad- 
hering particles  of  carbon  are  burnt,  then  place  the  filter  paper 
in  the  dish  and  ignite  over  a  full  flame  until  free  from  carbon.  (If 
fusion  takes  place,  either  the  time  of  lixiviation  has  not  been  long 
enough,  or  an  insufficient  amount  of  water  has  been  used  to  remove 
the  fusible  salts.)  Cool,  add  the  solution  from  the  beaker,  using 
as  little  water  as  possible  for  rinsing,  and  evaporate  to  dryness 
on  a  water  bath  or  Hillebrand  radiator.  Heat  carefully,  first  on 
the  radiator  or  in  a  drying  oven,  and  then  over  a  free  flame,  bring- 
ing the  ash  just  to  the  fusing  point,  then  cool  in  a  desiccator,  and 
weigh  as  rapidly  as  possible. 


I.       GENERAL   METHODS  11 

Ordinary  distilled  water  may  contain  enough  solids  to  cause 
an  appreciable  error  in  this  determination  where  the  amount  of  ash 
weighed  is  small,  as  in  the  case  of  cossettes  and  diffusion  juice. 
Water  of  as  high  a  degree  of  purity  as  possible  should  be  prepared 
by  redistillation  for  this  purpose,  and  the  results  should  be  cor- 
rected, if  necessary,  by  blank  tests  made  on  the  water. 

8.  ORGANIC  COEFFICIENT 

Calculate  by  either  of  the  following  methods: 

(a)  Add  together  the  percentages  of  raffinose,  invert  sugar, 
and  undetermined,  and  divide  by  the  percentage  of  ash   (all  per- 
cfii:ages  on  dry  substance). 

(b)  Add  together  the  percentages  of  sugar  by  inversion  and 
ash,  and  subtract  the  sum  from  100.     Divide  this  result  by  the  per- 
c enrage  of  ash  (all  percentages  on  dry  substance). 

9.  SULPHURIC  ACID  (SOS) 

Weigh  on  a  pulp  balance  20  grams  of  thick  juice,  sugar,  or 
saccharate  products,  and  in  the  case  of  other  products  more  or  less, 
depending  on  their  SO3  content.  Transfer  to  a  250  ml  beaker,  add 
about  150  ml  of  water  and  a  few  ml  of  hydrochloric  acid,  heat 
until  all  soluble  matter  is  dissolved,  filter  off  the  insoluble  matter. 
and  wash  with  hot  water.  Heat  to  boiling  and  add  slowly,  drop 
by  drop.  10  ml  of  a  hot  I0f/f  barium  chloride  solution.  After 
standing  for  at  least  three  hours,  filter,  wasli  with  hot  water,  dry. 
ignite,  and  weigh  as  BaSO4.  Test  the  filtrate  by  adding  a  few 
drops  of  barium  chloride.  Conduct  the  ignition  at  as  low  a  tem- 
P  rature  a--  possible  to  avoid  reduction  to  sulphide.  Heating  the 
crucible  in  an  inclined  position  will  reoxidize  any  sulphide  forme  ! 
TO  sulphate:  do  not  use  a  blast  lamp  as  too  high  a  temperature  will 
decompose  barium  sulphate.  Multiply  by  M430  to  convert  BaSl). 
8Og.  To  obtain  "SOa  per  100  Brix"  multiply  the  percentage 
of  SO  found  by  100  and  divide  by  the  Brix. 

10.     ALKALINITY 

Use  X  28  sulphuric  acid  (1  ml  =  .001  g  CaO)  for  juices, 
syrups,  etc..  and  nitric  acid  (1  ml  =  .05  g  CaO)  for  Steffen  liquors. 
Employ  phenolphthalein  as  indicator  in  all  cas< •>..  Qse  only  neutral 
water  for  all  dilutions. 


12  METHODS    OF    ANALYSTS 

(a)  JUICES 

Transfer  10  ml  with  a  pipette  to  a  porcelain  dish,  dilute  with 
neutral  water  if  dark,  add  a  few  drops  of  indicator  solution,  and 
add  the  standard  acid  until  the  pink  color  entirely  disappears ; 
test  for  the  end  point  by  adding  a  drop  of  the  indicator.  If  the 
solution  is  acid,  add  an  excess  of  N/28  sodium  hydroxide  solution, 
and  titrate  back  to  neutrality  with  the  standard  acid ;  subtract 
from  the  number  of  ml  of  alkali  added  the  number  of  ml  of  acid 
required.  In  the  case  of  highly  colored  products  where  it  is  diffi- 
cult to  observe  the  end  reaction,  transfer  10  ml  to  a  test  tube  or 
a  tumbler  and  dilute  with  about  50-100  ml  of  water:  fill  a  second 
vessel  in  the  same  manner.  Add  phenolphthalein  to  one  and  titrate 
with  the  standard  acid  until  a  color  match  for  the  two  solutions  is 
obtained. 

Express  the  result  as  "grams  of  CaO  p?r  100  ml,"  by  divulin.^ 
the  number  of  ml  of  acid  required  by  100.  Express  acidity  as 
negative  alkalinity  on  the  same  basis. 

( b )  MASSECUITE 

Use  10  ml  of  the  double  diluted  solution  prepared  for  the  Brix 
determination,  titrate  as  in  (a),  and  multiply  the  result  by  2. 

(c)  STEFFEN  LIQUORS 

Measure  out  50  ml  with  a  pipette,  add  a  few  drops  of  indicator, 
and  titrate  to  neutrality  with  the  standard  nitric  acid  ( 1  ml  =  .05 
g  CaO).  Express  the  result  as  "grams  of  CaO  p?r  100  ml"  by 
dividing  the  number  of  ml  of  acid  required  by  10. 


11.     CaO  BY  TITRATION 

Use  standard  nitric  acid  and  sodium  hydroxide  (1  ml  =  .0") 
g  CaO),  and  phenolphthalein  indicator. 

Dilute  the  weighed  sample  with  50-100  ml  of  neutral  water  in 
a  porcelain  casserole,  add  an  excess  of  the  standard  acid,  and  boil 
for  3-5  minutes  to  expel  all  carbon  dioxide.  (The  amount  of  dilu- 
tion and  time  of  boiling  must  be  maintained  within  the  p^e^ribod 
limits  in  order  to  drive  off  all  carbon  dioxide  produced  from  the 
decomposition  of  carbonates  and  at  the  same  time  not  to  volatilize 
any  nitric  acid.)  Add  a  few  drops  of  indicator  and  titrate  to 
neutrality  with  the  standard  alkali. 


I.      GENERAL  METHODS  13 

If  5  grams  of  the  sample  is  used  for  the  determination,  the 
number  of  ml  of  acid  used,  less  the  number  of  ml  of  alkali  required, 
gives  directly  the  percentage  of  calcium  oxide. 

12.     CaO  BY  SOAP  SOLUTION 

Use  a  soap  solution  prepared  and  standardized  as  described 
in  Chap.  XXV,  21,  and  adjusted  to  a  strength  of  1  ml  =  .001  g 
CaO  (twenty-eighth  normal). 

(a)  DETERMINATION  IN  THICK  JUICE,  SYRUPS,  MASSECUITE,  ETC 

Use  a  portion  of  the  23°  Brix  solution  prepared  for  the  ap- 
parent purity  determination.  Transfer  10  ml  with  a  pipette  to  an 
8  oz.  glass  bottle  provided  with  a  ground  stopper  and  marked  at 
the  point  at  which  it  holds  50  ml.  Fill  to  this  mark  with  water 
and  add  a  drop  of  phenolphthalein  solution.  If  the  reaction  is 
not  alkaline,  add  N/28  sodium  hydroxide  a  drop  at  a  time  until 
a  permanent  pink  color  is  produced.  Then  add  the  soap  solution 
in  small  quantities  from  a  burette;  after  each  addition  stopper  the 
bottle  and  shake  vigorously.  Take  as  the  end  point  the  formation 
of  a  fine  foam  5  mm  in  depth  which  will  last  five  minutes.  Make  a 
blank  test  on  each  lot  of  water  prepared  for  dilution,  first  adding 
phenolphthalein  and  then  N/28  sodium  hydroxide  a  drop  at  a  time 
until  a  permanent  pink  color  is  produced.  Subtract  from  the  num- 
ber of  ml  of  soap  solution  used  in  the  determination  the  number 
of  ml  of  soap  solution  required  by  40  ml  of  the  water  in  the  blank 
test.  Obtain  the  "CaO  to  100  Brix"  from  Table  15. 

The  quality  of  water  used  for  dilution  should  be  the  best  available,  in 
order  that  the  correction  may  be  kept  as  small  as  possible. 

The  recognition  of  the  end  point  is  a  matter  of  experience.  Usually 
a  granular  or  curdy  precipitate  is  formed  at  the  beginning  of  the  addi- 
tion of  the  soap  solution;  when  the  amount  of  this  is  large,  it  collects  on 
the  surface  and  may  be  mistaken  for  the  final  foam.  As  the  end  point 
is  approached,  the  precipitate  breaks  up  and  yields  a  uniformly  opaque 
solution.  Practice  will  enable  the  end  point  to  be  recognized  immediately 
by  the  fact  that,  as  long  as  the  bubbles  show  any  marked  sign  of  break- 
ing, the  amount  of  soap  solution  is  insufficient. 

(b)  DETERMINATION  IN  THIN  JUICES 

Determine  as  in  (a),  using  20  instead  of  10  ml  of  juice.  Cor- 
rect for  the  number  of  ml  of  soap  solution  required  by  30  ml  of 
the  water  in  the  blank  test.  Obtain  the  "CaO  to  100  Brix"  from 
Table  14. 


14  METHODS  OF  ANALYSIS 

13.     DETECTION  OF  SUGAR  BY  MEANS  OF  ALPHA- 
NAPHTHOL 

Employ  the  following  method  for  the  detection  of  sugar  in 
condensed  waters. 

Use  6x%  inch  test  tubes  graduated  at  %  inch  and  I1/*?  inches 
from  the  bottom.  Fill  the  tube  to  the  upper  mark  with  the  water 
under  examination,  add  5-10  drops  of  alpha-naphthol  solution,  and 
mix  thoroughly.  Cool  if  the  water  is  hot,  then  add  concentrated 
sulphuric  acid  (a  250  ml  dispensing  burette  is  convenient),  hold- 
ing the  tube  in  an  inclined  position  so  that  the  acid  will  run  lo 
the  bottom  and  form  a  separate  layer,  and  continuing  the  addition 
until  the  acid  layer  reaches  the  %  inch  mark. 

If  a  lilac  or  purple  ring  appears  at  the  intersection  of  the  two 
layers  during  the  addition  of  the  acid  or  immediately  thereafter, 
polarize  the  water  as  follows :  Cool  if  the  water  is  hot,  filter  if 
necessary,  and  read  directly  in  a  400  mm  tube  without  the  addition 
of  lead  acetate.  To  obtain  the  percentage  of  sugar  multiply  the 
reading  by  .13,  or  use  Table  8.  If  the  polariscope  reading  is  less 
than  .2,  record  as  a  "heavy  trace,"  which  should  represent  a  con- 
centration of  at  least  1  part  of  sugar  in  10,000  parts  of  water. 

If  the  color  does  not  appear  immediately  upon  the  addition 
of  the  acid,  roll  the  test  tube  once  in  an  upright  position  between 
the  palms  of  the  hands.  If  no  purple  or  lilac  ring  appears  within 
15  seconds,  report  sugar  as  absent.  If  the  characteristic  color  ap- 
pears within  this  time,  report  as  a  ' 'light  trace, ' '  which  should  sig- 
nify that  the  water  contains  from  1  part  of  sugar  in  10,000  to  1 
part  in  100,000. 

Previous  to  the  campaign  and  frequently  during  the  campaign, 
test  the  stock  of  alpha-naphthol  with  freshly  prepared  sugar  solu- 
tions of  known  concentration,  as  follows : 

Per  Cent  Sugar  Concentration 
1.0  1 :100 

.1  1 :1000 

.01  1  rlOOOO 

.001  1 :100000 

The  conditions  of  the  test  may  be  modified  accordingly,  if 
necessary.  Any  alpha-naphthol,  however,  which  is  not  sufficiently 
sensitive  to  give  a  reaction  in  a  1 : 100,000  sugar  solution  after  15 
seconds  standing  should  Joe  discarded  or  repurified.  Chemists 


I.      GENERAL  METHODS  15 

should  familiarize  themselves  with  the  shade  of  color  produced  by 
each  of  the  above  standard  sugar  solutions. 

The  following  resume  will  be  found  convenient  for  reference: 

Approximate 
Designation  Abbreviation  Percentage  of 

Sugar  Indicated 

Zero  0  Less  than  .001% 

Light  Trace  L  .001  to  .010% 

Heavy  Trace  H  .010  to  .026% 

A  figure  The  percent-age  indicated. 


II.     REGULAR  FACTORY  CONTROL 

1.     COSSETTES 


Determine : 


(a)  Sugar  every  hour. 

(b)  Apparent  Purity,  every  2  hours. 

(c)  Lixiviated  Ash,  every  24  hours. 

SAMPLING 

Fill  a  2-gallon  pail  by  holding  it  in  the  stream  of  cossettes  as 
they  fall  from  the  conveyor,  or  from  the  slicers.  Pay  particular 
attention  to  securing  a  sample  free  from  contamination  with  steam 
or  water.  See  also  below  under  * '  Tailings. ' ' 

As  a  check  upon  the  cossette  test,  an  extra  sample  should  be 
taken  every  2  hours  in  the  same  manner  as  the  regular  sample, 
but  at  a  different  time,  preferably  half  an  hour  before  or  after 
the  time  of  a  regular  sample.  The  sugar  should  be  determined 
by  a  different  operator  from  the  one  who  handles  the  regular 
samples. 

PREPARATION  OF  SAMPLE 

Grind  the  entire  sample  without  delay  in  an  Enterprise  Meat 
Chopper  No.  41  fitted  with  a  plate  containing  one-eighth  inch  per- 
forations and  running  at  the  rate  of  300  revolutions  per  minute. 
When  all  the  sample  has  been  introduced,  return  a  handful  of  the 
ground  material  to  the  machine  and  allow  the  machine  to  run  until 
no  more  material  or  juice  is  forced  through  the  perforated  plate. 
Do  not  add  to  the  sample  the  small  portion  of  the  material  remain- 
ing in  the  machine.  Mix  the  ground  sample  thoroughly  with  the 
hands,  take  out  a  small  portion  for  analysis,  and  place  it  in  a 
covered  bucket.  Use  the  remainder  of  the  ground  sample  for  the 
purity  determination.  After  the  sample  has  been  ground,  open 


II.      REGULAR  FACTORY  CONTROL  17 

the  machine  and  wash  it  out  well  with  hot  water.  Be  sure  that  it 
is  dry  before  it  is  used  again.  Use  this  machine  only  for  grinding 
cossettes. 

Obtain  the  juice  for  the  purity  determination  as  follows :  Place 
a  suitable  amount  of  the  ground  sample  in  a  clean,  dry  cloth  and 
subject  it  to  a  pressure  of  240  Ibs.  per  sq.  in.  in  a  hydraulic  press. 
Measure  the  pressure  with  a  suitable  high  pressure  gage;  the  gage 
pressure  to  be  carried  depends  on  the  dimensions  of  the  basket  and 
the  ram,  and  is  calculated  as  described  in  Chap.  XXIII,  14.  Bring 
up  the  pressure  gradually  and  maintain  the  prescribed  pressure 
until  juice  ceases  to  flow.  Collect  the  entire  amount  of  juice  ex- 
pressed and  mix  it  well.  Use  the  press  and  the  cloths  exclusively 
for  cossettes,  wash  them  well  with  hot  water  after  use,  and  see 
that  they  are  dry  before  they  are  used  again.  A  small  drying 
closet,  heated  by  steam  pipes,  should  be  employed  for  drying  cos- 
sette  and  pulp  cloths. 

ANALYSIS 

(a)  Sugar:  Weigh  out  26  grams  of  the  ground  cossettes  as 
rapidly  as  possible,  and  rinse  with  a  jet  of  water  into  a  200.6  ml 
Kohlrausch  flask.  Add  6  ml  of  basic  lead  acetate  solution  and 
sufficient  water  to  make  a  volume  of  about  160-170  ml.  Digest  in 
a  water  bath  at  80°,  keeping  the  body  of  the  flask  entirely  im- 
mersed but  not  in  contact  with  the  bottom  of  the  bath.  Remove 
the  flask  from  time  to  time  and  mix  with  a  rotary  motion.  At  the 
end  of  exactly  30  minutes  fill  to  the  mark,  or  slightly  above  it,  with 
water  at  80°  and  continue  the  digestion  for  exactly  10  minutes 
longer.  Then  cool  to  approximately  20°  in  a  cold  water  bath  and 
make  up  to  the  mark  with  the  necessary  small  amount  of  water. 
Use  a  few  drops  of  ether  to  break  the  foam,  adding  it  either 
just  previous  to  the  second  period  of  digestion  or  after  the  solu- 
tion has  been  cooled.  Shake,  filter,  and  polarize  in  a  400  mm  tube. 
The  reading  gives  directly  the  percentage  of  sugar. 

In  the  case  of  beets  of  abnormally  low  purity,  8-10  ml  of  basic 
lead  acetate  solution  may  be  needed  for  clarification. 

(b)  Apparent  Purity:  Place  the  juice  in  a  cylinder  under 
vacuum  until  all  air  has  been  removed  and  determine  as  described 
in  the  "General  Methods,"  4  (b).  Use  a  stronger  lead  solution  for 
clarification,  if  necessary,  and,  if  this  is  insufficient,  proceed  as 
follows :  Transfer  50  ml  with  a  pipette  to  a  100-110  ml  flask,  add 
sufficient  basic  lead  acetate  for  clarification,  and  make  up  to  the 


18  METHODS  OP  ANALYSIS 

110  ml  mark  with  water.  Multiply  the  polariscope  reading  by  2 
before  applying  the  formula  or  the  table.  The  use  of  the  last 
mentioned  method  should  very  seldom  be  necessary,  and  then  only 
in  the  case  of  beets  of  abnormally  low  purity. 

(c)  Lixiviated  Ash:  Weigh  out  5-10  grams  in  a  platinum 
dish  from  the  sample  of  ground  cossettes  used  for  one  of  the 
hourly  sugar  determinations  on  which  the  apparent  purity  is  also 
determined.  Follow  the  "General  Methods,"  7  (b). 

TAILINGS 

If  beet  tailings  are  introduced  and  pass  through  the  automatic 
scales  with  the  beets,  no  particular  attention  need  be  paid  to  them, 
as  the  cossette  samples  will,  in  the  long  run,  include  a  proportional 
amount  of  the  tailings. 

If  tailings  are  introduced  which  do  not  pass  through  the  auto- 
matic scales,  they  may  be  handled  by  one  of  the  following  methods : 

(1)  If  the  tailings  are  mixed  with  the  cossettes  at  a  reason- 
ably uniform  rate,  take  the  cossette  samples  as  above,  so 
that  they  will  include  a  proportional  amount  of  the  tail- 
ings.    Add   the   weight   of   tailings  introduced   to   the 
weight  of  beets  which  passes  through  the  scales. 

(2)  Take  the  cossette  samples  at  a  point  where  none  of  the 
tailings  will  be  included  in  the  sample ;  sample  the  tail- 
ings also  once  a  shift,  grind,  and  determine  the  percent- 
age of  sugar  as  in  the  case  of  "Cossettes."     Add  the 
"equivalent  in  beets"  of  the  weight  of  tailings  to  the 
weight  of  beets  which  passes  through  the  scales. 

In  either  of  the  preceding  two  cases  determine  the  amount  of  tail- 
ings introduced  by  actual  weighing  for  a  24  hour  period  at  least 
once  a  week. 

2.     DIFFUSION  JUICE 

Determine  every  2  hours : 

(a)  Brix. 

(b)  Apparent  Purity. 

Determine  every  24  hours: 

(c)  Lixiviated  Ash. 


II.   REGULAR  FACTORY  CONTROL  19 

SAMPLING 

Take  a  catch  sample  from  a  full  measuring  tank,  or  from  the 
pipe  line  or  pump  before  the  juice  enters  the  heaters. 

ANALYSIS 

(a)  Brix:    Follow  the  " General  Methods,"  I  (a). 

(b)  Apparent  Purity:     Determine  as  in    (b)    under  "Cos- 
settes." 

(c)  Lixiviated  Ash:     Weigh  out  7-10  grams  of  one  of  the 
catch  samples  and  proceed  as  in  the  " General  Methods,"  7   (b). 

SPECIAL  DETERMINATIONS 

(d)  Acidity:     Measure  out  10  ml  in  a  porcelain  dish,  add 
two  or  three  times  its  volume  of  neutral  water  to  lighten  the  color, 
and  a  few  drops  of  phenolphthalein.     Add  an  excess  of  standard 
sodium  hydroxide  (1  ml  =  .001  g  CaO),  then  titrate  to  neutrality 
with  standard  sulphuric  acid  of  the  same  strength.     Express  the 
result  in  grams  of  CaO  per  100  ml.     See  "General  Methods," 
10  (a). 

(e)  Invert  Sugar:    Use  one  of  the  samples  on  which  the  pre- 
vious determinations  have  been  made,  but  do  not  allow  it  to  stand 
for  any  length  of  time  before  starting  this  determination.     Follow 
the  "General  Methods,"  6  (b). 

3.     PULP  AND  PULP  WATER 

Determine  hourly  in  a  sample  from  each  diffusion  battery: 
(a)     Sugar. 

SAMPLING 

The  workman  under  the  battery  should  take  from  each  cell 
dumped  a  small  portion  of  the  mixture  of  pulp  and  pulp  water, 
using  a  long  handled  dipper.  The  sample  should  be  taken  from 
the  first  pulp  and  water  discharged.  The  individual  sample  should 
be  transferred  at  the  time  to  a  covered  container  of  the  customary 
type,  so  arranged  that  the  water  will  drain  into  the  bottom  of 
the  receptacle  and  not  stand  in  contact  with  the  pulp. 

PREPARATION  OP  SAMPLE 

Grind  the  entire  sample  of  pulp  in  an  Enterprise  Meat  Chop- 
per No.  41  in  the  same  manner  as  described  under  "1.  Cossettes," 


20  METHODS  OF  ANALYSIS 

and  press  in  a  clean,  dry  cloth  in  a  suitable  hand  press.  Collect 
the  entire  amount  of  juice  that  can  be  expressed  and  mix  it  well. 
Keep  the  grinding  machine,  press,  and  cloths  clean,  and  use  them 
only  for  pulp. 

ANALYSIS 

(a)  Sugar:  Measure  out  100  ml  of  the  expressed  juice  in 
a  100-110  ml  flask,  add  2-4  ml  of  basic  lead  acetate  solution,  fill 
to  the  110  ml  mark  with  water,  shake,  filter,  and  polarize  in  a  200 
mm  tube.  Obtain  the  percentage  of  sugar  from  Table  6.  Analyze 
the  pulp  water  in  the  same  way,  using  1-2  ml  of  lead  acetate. 

4.     FLUME  PULP  AND  PULP  WATER 

Determine  every  2  hours: 
(a)     Sugar. 

SAMPLING 

The  sample  should  be  taken  by  a  laboratory  employe  and 
should  be  as  nearly  representative  as  possible  of  the  pulp  leaving 
the  battery  at  the  time.  Obtain  the  sample  from  the  discharge  of 
the  pit,  from  the  flume  leading  to  the  pump,  or  from  the  return  line 
of  the  pump,  using  a  long  handled  dipper.  Take  the  sample  while 
a  good  sized  stream  of  pulp  is  flowing  in  order  to  avoid  excessive 
admixture  of  washout  water,  transferring  it  to  the  same  kind  of 
container  which  is  used  for  the  regular  pulp  samples. 

PREPARATION  OF  SAMPLE 

Grind  and  prepare  the  sample  in  the  same  manner  as  the 
regular  pulp  sample. 

ANALYSIS 

(a)  Sugar:  Determine  the  sugar  in  the  pulp  and  the  water 
in  the  same  manner  as  in  the  regular  pulp  and  pulp  water  samples. 

5.    FIRST  SATURATION  JUICE 

Determine  every  hour  on  a  catch  sample : 
(a)     Alkalinity. 


II.      REGULAR  FACTORY  CONTROL  21 

Determine  every  4  hours  on  a  composite  sample : 

(b)  Brix. 

(c)  Apparent  Purity. 

SAMPLING 

Take  a  catch  sample  every  hour  from  the  cocks  or  troughs  of 
the  first  presses,  avoiding  any  admixture  of  wash  water.  Make 
up  the  composite  sample  by  mixing  equal  portions  of  the  four 
hourly  samples.  Keep  the  container  for  the  composite  sample 
clean,  and  add  a  few  drops  of  formaldehyde  to  prevent  decom- 
position. 

ANALYSIS 

(a)  Alkalinity:    Follow  the  "General  Methods,"  10  (a). 

(b)  Brix:    Follow  the  "General  Methods,"  1  (a),  using  the 
original  juice,  and  not  the  carbonated  sample  described  in    (c) 
below. 

(c)  Apparent  Purity:    Heat  to  80°  in  a  water  bath  and  car- 
bonate at  this  temperature  to  faint  alkalinity  with  phenolphthalein. 
Then  heat  to  at  least  85°,  filter,  cool,  redetermine  the  Brix,  and 
determine  the  apparent  purity  according  to  the  "General  Meth- 
ods," 4  (b). 

NOTE:  When  the  melted  sugar  is  added  at  the  blow-ups  or 
at  a  point  beyond  the  second  saturation,  a  composite  sample  of 
Second  Saturation  Juice  may  be  used  for  the  apparent  purity 
determination  without  laboratory  carbonation 

6.     SECOND  AND  THIRD  SATURATION  JUICE 

Determine  every  hour  on  a  catch  sample : 

(a)  Alkalinity. 

Determine  every  4  hours  on  a  composite  sample : 

(b)  Brix. 

SAMPLING 

Take  a  catch  sample  every  hour  from  the  cocks  or  troughs  of 
the  respective  filters,  avoiding  any  admixture  of  wash  water.  Make 
up  the  composite  sample  by  mixing  equal  portions  of  the  four 
hourly  samples.  Keep  the  containers  for  the  composite  samples 


22  METHODS  OF  ANALYSIS 

clean,  and  add  a  few  drops  of  formaldehyde  to  prevent  decom- 
position. 

ANALYSIS 

Follow  the  "General  Methods,"  10  (a)  and  1  (a). 

7.     EVAPORATOR  THIN  JUICE 

Determine  every  4  hours  on  a  composite  sample : 

(a)  Brix. 

(b)  Apparent  Purity. 

(c)  Lime  Salts  (CaO  to  100  Brix). 

SAMPLING 

Take  a  catch  sample  every  hour  from  the  pump,  or  at  a  suit- 
able point  in  the  pipe  line  between  the  thin  juice  filters  and  the 
first  body  of  the  evaporators.  Make  up  the  composite  sample  by 
mixing  equal  portions  of  the  four  hourly  samples.  Keep  the  con- 
tainer for  the  composite  sample  clean,  and  add  a  few  drops  of 
formaldehyde  to  prevent  decomposition. 

ANALYSIS 

Follow  the  "General  Methods,"  1  (a),  4  (b),  and  12  (b). 
Add  1-2  ml  of  alumina  cream  before  making  up  to  the  mark,  if 
trouble  is  encountered  in  obtaining  a  clear  filtrate. 

8.     EVAPORATOR  THICK  JUICE. 

Determine  every  hour  on  a  catch  sample : 

(a)  Alkalinity. 

Determine  every  4  hours  on  a  composite  sample : 

(b)  Brix. 

(c)  Apparent  Purity. 

(d)  Lime  Salts  (CaO  to  100  Brix). 

SAMPLING 

Take  a  sample  every  hour  from  the  pump,  or  from  the  line 
between  the  evaporator  outlet  and  the  blow-up  inlet.  Do  not  take 


II.      REGULAR  FACTORY  CONTROL  23 

the  sample  from  the  last  body  of  the  evaporators,  because  the 
sample  so  drawn  is  not  always  representative  of  the  juice  leaving 
the  evaporators.  Make  up  the  composite  sample  by  mixing  equal 
portions  of  the  four  hourly  samples. 

ANALYSIS 

(a)     AIM h)  if  it  and   (b)   Brix:     Follow  the  "  General  Meth- 
ods," 10   (a)   and  1   (a). 

(c)  Apparent  Purity:   Dilute  to  the  approximate  density  of 
the  evaporator  thin  juice  and  determine  according  to  "General 
Methods,"  4  (b).    The  dilution  is  prescribed  in  this  case  in  order 
to  eliminate  the  small  variation  in  the  purity  test  which  would  be 
caused  if  the  thin   and  thick  juice  were   analyzed   at  different 
densities. 

(d)  Lime  Salts  (CaO  to  100  Brix):    Use  20  ml  of  the  solu- 
tion diluted  to  thin  juice  density  as  in  (c),  and  follow  the  "Gen- 
eral Methods"  for  the  determination  of  CaO  by  Soap  Solution  in 
linn  juices,  12  (b). 

9.     BLOW-UP  THICK  JUICE 

Determine  every  hour  on  a  catch  sample: 

(a)  Alkalinity. 

Determine  every  4  hours  on  a  composite  sample : 

(b)  Lime  Salts  (CaO  to  100  Brix). 

SAMPLING 

Take  a  catch  sample  every  hour  from  the  cocks  or  troughs  of 
the  thick  juice  filters.  Make  up  the  composite  sample  by  mixing 
equal  portions  of  the  four  hourly  samples. 

ANALYSIS 

(a)  All-nlnnfj,;    Follow  the  "General  Methods,"  10  (a). 

(b)  Lime  Salts  (CaO  to  100  Brix) :    Dilute  to  approximately 
23°  Brix,  determine  the  Brix,  and  use  10  ml,  following  the  "Gen- 
eral Methods,"  12  (a).    Or  dilute  to  thin  juice  density,  determine 
the  Brix,  and  use  20  ml,  following  the  "General  Methods,"  12  (b). 

10.     LIME  KILN  GAS 
Determine  every  4  hours  : 

(a)     Carbon  dioxide  (C02). 


24  METHODS  OF  ANALYSIS 

(b)  Oxygen  (0). 

(c)  Carbon  monoxide  (CO). 

SAMPLING 

Obtain  the  gas  by  means  of  a  pipe  leading  to  the  laboratory 
from  a  point  in  the  main  gas  line  between  the  gas  washer  and  the 
carbonators.  Provide  the  laboratory  line  with  a  vent  leading  out- 
side the  building  by  means  of  which  the  line  may  be  exhausted  and 
kept  filled  with  fresh  gas. 

ANALYSIS 

Use  an  Orsat  apparatus  provided  with  three  pipettes  and  a 
water  jacketed  burette.  First  make  sure  that  the  vent  line  has 
been  open  for  several  minutes,  to  insure  a  supply  of  fresh  gas. 
Fill  the  Orsat  burette  with  water  by  raising  the  leveling  bottle, 
then  put  it  into  communication  with  the  gas  supply,  lower  the  level- 
ing bottle  below  the  zero  point  of  the  burette,  and  allow  the  gas 
to  fill  the  burette.  Then  expel  the  gas  sample  and  draw  in  another 
in  the  same  manner,  to  rinse  out  connections,  etc.,  or  allow  the 
gas  to  bubble  for  a  few  moments  through  the  water  in  the  leveling 
bottle;  in  the  latter  case  be  sure  that  no  gas  is  left  trapped  in 
the  rubber  tube  between  the  burette  and  the  leveling  bottle.  Put 
the  three-way  cock  into  communication  with  the  atmosphere,  at 
the  same  time  raising  the  leveling  bottle  until  the  level  of  the 
water  in  it  is  at  the  level  of  the  zero  point  on  the  burette.  When 
equilibrium  has  been  reached,  i.  e.,  when  the  water  in  the  burette 
has  reached  the  zero  mark  while  the  water  in  the  bottle  is  at  the 
same  level,  the  apparatus  contains  100  ml  of  gas  measured  at 
atmospheric  pressure;  turn  the  three-way  cock  so  that  no  gas 
can  enter  or  leave  the  apparatus.  Be  careful  never  to  allow  the 
level  of  the  water  in  the  burette  to  fall  while  the  three-way  cock 
is  open  to  the  atmosphere,  otherwise  air  will  be  drawn  into  the 
apparatus  which  will  dilute  the  gas  and  render  the  analysis  inac- 
curate. Raise  the  leveling  bottle,  open  the  stopcock  of  the  first 
absorption  pipette,  and  force  the  greater  part  of  the  gas  into  it, 
then  lower  the  bottle  and  draw  most  of  the  gas  back  into  the 
burette.  Repeat  this  twice,  the  last  time  bringing  the  absorption 
liquid  to  the  mark  on  the  absorption  pipette,  then  close  the  stop- 
cock. Bring  the  leveling  bottle  to  the  point  where  its  water  level 
corresponds  to  that  of  the  burette,  then  read  off  the  percentage 
of  carbon  dioxide.  Repeat  the  absorption  process  until  the  vari- 
ation is  not  over  0.2%. 


II.      REGULAR  FACTORY  CONTROL  25 

Absorb  the  oxygen  and  carbon  monoxide  in  a  similar  manner  in 
the  other  two  pipettes,  obtaining  the  percentages  by  difference. 

Renew  the  solutions  in  the  absorption  pipettes  every  two 
weeks,  or  as  often  as  is  found  to  be  necessary.  See  Chap.  XXV, 
14,  regarding  the  preparation  of  the  absorption  solutions. 

11.     DIME  TO  SLACKER 

Determine  every  24  hours: 
(a)     CaO  by  Titration. 

SAMPLING 

Obtain  a  one-pint  sample  every  2  hours,  from  the  pile  of  lime 
from  which  the  slacker  is  being  fed,  by  breaking  off  small  pieces, 
approximately  one  inch  cubes.  In  taking  the  sample  reject  such 
material  as  sand,  coke,  unburned  limestone,  etc.,  which  will  be 
eliminated  in  the  form  of  discard  from  the  slacker.  Keep  the 
samples  sealed  and  in  a  dry  place. 

PREPARATION  OP  SAMPLE 

Crush  the  twelve  pints  representing  the  average  sample  for 
the  24  hours  to  one-quarter  inch  size  in  a  jaw  crusher,  mix  and 
quarter,  repeating  the  mixing  and  quartering  until  the  sample  is 
reduced  to  about  one  pint.  Grind  this  sample  to  60  mesh  on  a 
bucking  board  or  in  a  disc  pulverizer.  Mix  the  60  mesh  material 
and  fill  a  four  ounce  bottle  by  taking  small  portions  from  various 
parts  of  the  sample.  Seal  this  sample  and  take  it  to  the  laboratory. 
Handle  the  lime  as  rapidly  as  possible  during  the  preparation  of 
the  sample  to  avoid  absorption  of  moisture. 

ANALYSIS 

Determine  the  CaO  by  Titration,  according  to  the  "General 
Methods,"  Chap.  I,  11. 

12.     MILK  OF  LIME 

Determine  every  hour : 

(a)  Brix. 

(b)  CaO  (grams  in  100  ml). 


26  METHODS  OP  ANALYSIS 

SAMPLING 

Take  a  catch  sample  from  the  discharge  line  of  the  pump. 

ANALYSIS 

(a)  Brix:     Cool  under  vacuum,  mix  by  inverting  the  cylin- 
der gently  a  few  times,  and  determine  the  Brix  in  the  regular 
manner,  obtaining  the  reading  immediately  after  mixing  before 
the  insoluble  material  has  had  time  to  settle. 

(b)  CaO:    Measure  out  10  ml  of  the  cooled  liquid  with  a 
pipette  into  a  porcelain  casserole.     Add  50-100  ml  of  water  and 
proceed  as  in  the  "General  Methods,"  11.    Subtract  the  number  of 
ml  of  alkali  from  the  number  of  ml  of  acid  used,  and  divide  by  2. 

13.     LIME  CAKE,  FIRST  PRESSES 

Determine  every  3  hours : 

(a)  Total  Sugar. 

(b)  Free  Sugar. 

(c)  CaO. 

(d)  Sugar  to  100  CaO. 

SAMPLING  (PLATE  AND  FRAME  PRESSES) 

All  samples  are  to  be  taken  by  a  laboratory  employe,  who 
should  receive  the  following  instructions: 

(1)  Visit  the  press  floor  at  irregular  intervals. 

(2)  Sample  any  press  or  presses  which  are  being  dumped. 

(3)  As  a  rule,  do  not  sample  a  press  the  washing  of  which  is 
finished  while  the  employe  is  on  the  press  floor. 

(4)  Use  a  special  closed  can  provided  with  a  tube  which  cuts 
a  plug  one  inch  in  diameter  from  the  cake. 

(5)  Sample  several  frames  selected  at  random  in  each  press. 

(6)  Distribute  the  points  in  each  frame  where  samples  are 
taken  equally  over  the  face  of  the  cake,  taking  one  plug  from  each 
corner  and  one  from  the  middle  of  the  frame. 

(7)  At  least  five  presses  shall  enter  into  each  sample  taken 
to  the  laboratory  for  analysis. 

NOTE:  If  conditions  warrant  it,  a  man  under  laboratory 
supervision  should  be  stationed  permanently  on  the  press  floor 
so  that  all  presses  dumped  may  be  sampled. 


II.     REGULAR  FACTORY  CONTROL  27 

SAMPLING  (KELLY  PRESSES) 

Where  the  manner  of  installation  permits,  catch  a  portion  of 
the  cake  discharged  from  each  frame  by  laying  a  board  diagonally 
across  the  hopper  before  the  press  is  opened,  placing  one  end  of 
the  board  flush  against  a  corner  of  the  hopper  near  the  press  in 
order  that  a  small  portion  of  any  cake  which  may  have  fallen  off 
into  the  drum  and  may  not  have  been  properly  washed  may  be 
included  in  the  sample.  When  the  press  has  been  emptied,  obtain 
an  average  sample  of  the  material  on  the  board  by  means  of  a 
sampling  device  of  the  kind  used  for  sampling  plate  and  frame 
presses,  or  by  means  of  a  piece  of  tubing  about  l1^  inches  in 
diameter. 

Where  the  presses  are  set  too  low  to  admit  of  the  board  being 
used,  employ  a  rectangular  metal  box  attached  to  a  long  curved 
handle,  the  whole  of  rigid  construction,  by  means  of  which  sam- 
ples may  be  caught  underneath  the  several  frames  as  the  cake 
drops  off;  preserve  the  various  samples  taken  in  a  covered  con- 
tainer. In  catching  the  samples  be  careful  to  avoid  any  water 
from  the  hose  used  for  washing  the  cake  off  the  frames. 

If  an  appreciable  amount  of  cake  falls  off  into  the  drum,  en- 
deavor to  include  a  proportionate  amount  of  this  in  the  sample. 
Follow  also  the  general  instructions  under  "  Sampling  (Plate  and 
Frame  Presses)  "  as  far  as  they  can  be  made  to  apply  to  Kelly 
presses,  but  do  not  under  any  circumstances  obtain  the  sample 
by  scraping  the  cake  from  the  sides  of  the  outer  frames  or  from 
the  top  of  the  several  frames. 

PREPARATION  OF  SAMPLE 

Transfer  the  entire  sample  to  a  large  iron  mortar  and  mix 
thoroughly  with  an  iron  pestle. 

ANALYSIS 

(a)  Total  Sugar — Method  I:  Weigh  out  53  grams  in  a 
counterpoised  Monel  metal  cup,  or  " capsule,"  of  about  350  ml 
capacity.  Add  from  an  automatic  pipette  177  ml  of  a  10%  solu- 
tion of  commercial  zinc  nitrate.  Put  in  a  piece  of  metal  chain, 
cover  with  an  aluminum  disc  enclosed  in  a  rubber  envelope,  and 
shake  vigorously  until  the  cake  has  been  completely  disintegrated. 
Filter  and  polarize  in  a  200  mm  tube.  The  reading  gives  directly 
the  percentage  of  total  sugar. 

Total  Sugar — Method  II:  Weigh  out  54  grams  in  a  counter- 
poised metal  cup  and  add  slowly  177  ml  of  dilute  acetic  acid  (see 


28  METHODS  OF  ANALYSIS 

Chap.  XXV,  1),  stirring  with  a  glass  rod  until  most  of  the  foam- 
ing has  ceased.  Put  in  a  piece  of  metal  chain,  cover,  and  shake  as 
in  the  previous  method.  Then  add  3  ml  of  basic  lead  acetate 
solution,  shake  again,  filter,  and  polarize  in  a  200  mm  tube.  The 
reading  gives  directly  the  percentage  of  total  sugar. 

(b)  Free  Sugar — Method  I:    Weigh  out  53  grams  and  de- 
termine as  in  "Total  Sugar — Method  I,"  adding,  in  place  of  the 
zinc  nitrate  solution,   177  ml  of  water  containing  3  ml  of  lead 
acetate  in  each  177  ml. 

Free  Sugar — Method  II:  Weigh  out  54  grams,  and  determine 
as  in  "Total  Sugar — Method  II,"  adding  177  ml  of  water  without 
any  acetic  acid,  followed  by  3  ml  of  lead  acetate. 

(c)  CaO:    Weigh  out  5  grams  and  proceed  as  in  the  "Gen- 
eral Methods,"  11. 

(d)  Sugar  to  100  CaO:     Multiply  the  percentage  of  total 
sugar  by  100  and  divide  by  the  percentage  of  CaO. 

14.    LIME  CAKE,  SECOND  PRESSES 

Determine  every  8  hours: 

(a)  Total  Sugar. 

(b)  CaO. 

SAMPLING  AND  PREPARATION  OF  SAMPLE 

Take  and  prepare  the  sample  in  the  same  manner  as  the  first 
lime  cake. 

ANALYSIS 

Determine  total  sugar  and  CaO  in  the  same  manner  as  in  the 
first  lime  cake. 

15.     LIME  SEWER 

Determine  every  2  hours : 

(a)  Total  Sugar. 

(b)  CaO. 

(c)  Sugar  to  100  CaO. 

SAMPLING 

Obtain  a  continuous  sample  if  a  suitable  device  is  available. 
In  the  absence  of  this  take  a  catch  sample  at  least  every  hour  from 


II.      REGULAR  FACTORY  CONTROL  29 

the  mud  mixer,  or,  in  the  absence  of  a  mud  mixer,  at  some  point 
in  the  line  leading  to  the  sewer,  or  if  possible  at  the  point  of  dis- 
charge into  the  sewer.  Mix  the  sample  thoroughly  until  any  lumps 
are  broken  up,  and  take  a  portion  to  the  laboratory.  Make  up 
a  composite  sample  every  2  hours. 

ANALYSIS 

If  the  material  is  thin  enough  to  measure  readily,  use  Method 
II  for  total  sugar.  If  the  material  is  thick,  use  Method  I. 

(a)  Total  Sugar — Method  I:    Mix  the  sample  well,  and  de- 
termine as  in  the  case  of  "Lime  Cake,  First  Presses,"  Method  I 
or  Method  II. 

Total  Sugar — Method  II:  Mix  the  sample  well,  measure  out 
100  ml  in  a  100-110  ml  flask,  add  a  few  drops  of  phenolphthalein 
and  neutralize  with  acetic  acid.  Add  3  ml  of  lead  acetate,  make  up 
to  the  110  ml  mark  with  water,  shake,  filter,  and  polarize  in  a  200 
mm  tube.  Obtain  the  "grams  of  sugar  in  100  ml"  from  Table  6. 

(b)  CaO:    If  the  total  sugar  has  been  determined  by  taking 
a  definite  weight  of  the  material,  mix  the  sample  well,  weigh  out 
10  grams,  and  determine  as  in  the  case  of  "Lime  Cake,   First 
Presses. ' '     Subtract  the  number  of  ml  of  alkali  from  the  number 
of  ml  of  acid  used,  and  divide  by  2. 

If  the  total  sugar  has  been  determined  by  measuring  out  a 
definite  volume,  use  10  ml,  or  a  multiple  thereof,  and  determine 
as  in  the  case  of  "Lime  Cake,  First  Presses."  If  10  ml  is  used, 
subtract  the  number  of  ml  of  alkali  from  the  number  of  ml  of 
acid  used,  and  divide  by  2. 

(c)  Sugar  to  100  CaO:     Multiply  the  percentage  of  total 
sugar  by  100  and  divide  by  the  percentage  of  CaO. 

16.     EXCESS  WATER 

Determine  every  4  hours: 

(a)  Brix. 

(b)  Total  Sugar. 

SAMPLING 

Obtain  the  sample  from  the  excess  water  tank  or  pump. 


30  METHODS  OF  ANALYSIS 

ANALYSIS 

(a)  Brix:    Follow  the  " General  Methods,"  1   (a). 

(b)  Total  Sugar:    Determine  as  in  the  case  of  "Lime  Sewer, 

Total  Sugar— Method  II." 

17.    SWEET  WATER. 

Determine  every  4  hours  on  a  catch  sample : 

(a)  Brix. 

Determine  every  8  hours  on  a  catch  sample : 

(b)  Apparent  Purity. 

(c)  Lime  Salts  (CaO  to  100  Brix). 

SAMPLING 

Take  a  catch  sample  from  the  sweet  water  tank  every  4  hours. 

ANALYSIS 

(a)  Brix:    Follow  the  "General  Methods,"  1  (a). 

(b)  Apparent   Purity:     Evaporate    to    approximately   thin 
juice  density,  and  carbonate  and  proceed  as  in  the  case  of  "5. 
First  Saturation  Juice." 

(c)  Lime  Salts  (CaO  to  100  Brix) :    Use  the  carbonated  solu- 
tion prepared  for  the  apparent  purity  determination,  and  follow 
the  "General  Methods,"  12  (b). 

18.     FILTER  CLOTH  WASH  WATER 

Determine  every  8  hours: 
(a)     Sugar. 

SAMPLING 

Take  a  small  sample  from  each  tank  or  washing  machine 
emptied  to  the  sewer,  and  keep  in  a  covered  container.  Do  not 
include  in  the  sample  any  water  returned  to  the  process. 

ANALYSIS 

Mix  well  and  determine  as  in  the  case  of  "Lime  Sewer,  Total 
Sugar  Method  II." 


n.      REGULAR  FACTORY  CONTROL  31 

19.     MAIN  SEWER 

Determine  every  2  hours: 
(a)     Sugar. 

SAMPLING 

Take  a  catch  sample  every  2  hours  at  a  point  where  it  will 
represent  all  sewer  water  leaving  the  main  factory,  but  avoiding 
the  pulp  silo  drainage  if  possible.  Or  take  more  frequent  samples 
and  composite  every  2  hours. 

ANALYSIS 

Mix  well  and  determine  as  in  the  case  of  "Lime  Sewer,  Total 
Sugar — Method  II."  Polarize  in  a  400  mm  tube  and  obtain  the 
percentage  of  sugar  from  Table  7. 

20.  WHITE  PAN  STORAGE  TANKS 

Determine  at  least  every  8  hours : 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Apparent  Purity. 

SAMPLING 

Take  samples  from  each  tank  on  the  pan  floor  at  the  beginning 
of  every  shift.  Special  samples  sent  to  the  laboratory  at  any  time 
during  the  shift  may  be  used  in  lieu  of  these  samples. 

ANALYSIS 

Follow  the  "General  Methods." 

21.    WHITE  MASSECUITE 

Determine  on  every  pan  dropped : 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Apparent  Purity. 

(d)  Lime  Salts  (CaO  to  100  Brix). 


32  METHODS  OF  ANALYSIS 

SAMPLING 

Take  the  sample  from  the  pan  or  from  the  spout  leading  to 
the  mixer  before  the  pan  is  steamed  out. 

ANALYSIS 

Follow  the  "General  Methods." 

22.     HIGH  GREEN  AND  WASH  SYRUPS 

Determine  either  once  or  twice  during  the  spinning  of  every  pan, 
or  at  regular  intervals  of  every  2  hours : 
(a)     Apparent  Purity. 

SAMPLING 

Take  the  samples  from  the  machine  receiving  tanks  where 
such  tanks  are  in  use,  otherwise  from  the  troughs  leading  from  the 
machine  spouts  to  the  pumps,  or  from  the  pumps.  Whenever 
possible  obtain  samples  that  have  been  mixed  by  steam.  Do  not 
take  the  samples  from  the  machine  spouts. 

ANALYSIS 

Follow  the  "General  Methods." 

23.     MOISTURE  IN  WHITE  SUGAR 

Determine  moisture  every  8  hours  in  the  following  samples: 

(1)  Wet  Sugar. 

(2)  Sugar  leaving  upper  granulator. 

(3)  Standard  granulated. 

(4)  Table  granulated. 

SAMPLING 

•  Provide  a  sufficient  number  of  1  x  3  inch  test  tubes  and  rubber 
stoppers;  it  is  advisable  to  heat  both  the  test  tubes  and  stoppers 
in  a  drying  oven  to  make  sure  that  they  are  perfectly  dry.  Sample 
each  kind  of  sugar  every  2  hours  by  filling  a  test  tube,  and  stopper 
immediately.  Make  up  a  composite  sample  every  8  hours  for  each 
kind  of  sugar  sampled  by  emptying  the  four  individual  samples 
into  a  wide  mouth,  glass  stoppered  bottle  and  mixing  thoroughly. 


II.      REGULAR  FACTORY  CONTROL  33 

Obtain  the  wet  sugar  from  the  discharge  into  the  wet  box  or 
from  the  feed  of  the  wet  box  to  the  upper  granulator.  Sample 
the  "sugar  leaving  upper  granulator"  at  the  discharge  from  the 
upper  to  the  lower  granulator.  Obtain  the  Standard  and  Table 
granulated  at  the  discharge  from  the  dry  boxes  into  the  bag.  If 
the  factory  has  only  a  single  granulator  system,  omit  sample  (2). 
ANALYSIS  . 

Place  approximately  fj  grains  in  the  case  of  wet  sugar,  and 
10  grams  in  the  case  of  granulated,  in  a  2  x  1%  inch  aluminum 
dish  provided  with  a  cover,  which  has  been  previously  dried  at 
100-105°.  Cover  the  dish,  and  weigh  accurately,  but  as  rapidly  as 
possible,  on  an  analytical  balance.  Remove  the  cover  and  dry  at 
100-105°  in  a  glycerin  oven  for  5  hours.  Replace  the  cover,  cool 
in  a  desiccator  over  sulphuric  acid,  and  weigh.  Keep  thermometers 
in  the  desiccator  and  balance  case,  and  do  not  make  the  weighings 
until  the  difference  in  temperature  is  2°  or  less.  The  loss  in  weight 
after  5  hours  heating  is  considered  to  represent  the  amount  of 
moisture. 

NOTE:  The  concentrated  sulphuric  acid  in  the  desiccator 
must  be  renewed  once  every  week,  experience  having  shown  that 
sugar,  after  drying  for  5  hours  or  more,  is  capable  of  absorbing 
n-tih  ,•  from  strong  acid  after  it  has  become  diluted  with  small 
amounts  of  moisture.  The  acid  should  be  renewed  also  at  any  time 
u'Jii'n  it  becomes  discolored  from  contamination  with  organic  mat- 
The  cover  of  the  desiccator  should  be  frequently  cleaned  and 
coated  with  fresh  vaseline. 

24.     PERCOLATION  TESTS  OF  WHITE  SUGAR 

If  the  white  sugar  is  not  up  to  standard,  make  percolation 
tests  occasionally  to  obtain  an  approximate  idea  of  how  much  of 
the  color  is  due  to  adhering  syrup  which  should  have  been  washed 
out  in  the  centrifugal  machines. 

Close  the  bottom  of  a  one-pint  Oldberg  percolator  with  a 
loosely  fitting  cotton  plug,  put  in  250  grams  of  sugar  and  add  250 
ml  of  distilled  water.  Catch  the  percolate  in  1  x  6  inch  text  tubes 
in  four  or  five  successive  portions,  and  compare  the  color  of  the 
solutions. 


25.     DUST  BOX 


Determine  every  8  hours: 
(a)     Brix. 


34  METHODS  OF  ANALYSIS 

(b)  Alkalinity. 

(c)  Apparent  Purity. 

SAMPLING 

Take  a  catch  sample  of  the  liquid  in  the  dust  box. 

ANALYSIS 

Follow  the  "General  Methods." 

26.     REMELT  PAN  STORAGE   TANKS 

Determine  at  least  every  8  hours: 

(a)  Brix. 

(b)  Apparent  Purity. 

SAMPLING 

See  "White  Pan  Storage  Tanks." 

ANALYSIS 

Follow  the  "General  Methods." 

27.     REMELT  MASSE  CUITE  FROM  PAN 

Determine  on  every  pan  dropped: 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Apparent  Purity. 

(d)  Lime  Salts  (CaO  to  100  Brix). 
Determine  every  24  hours : 

(e)  True  Purity. 

(f)  Raffinose  (%  on  dry  substance). 

SAMPLING 

Take  the  sample  from  the  pan  or  from  the  trough  leading 
to  the  crystallizers  before  the  pan  is  steamed  out. 

ANALYSIS 

Follow  the  "General  Methods."  Obtain  the  dry  substance  for 
the  true  purity  determination  either  by  the  refractometer  or  by 
oven  drying. 


II.      REGULAU  FACTORY  CONTROL  35 

28.     EEMELT  MASSECUITE  FROM  CRYSTALLIZEB. 

Determine  on  every  crystallizer  dropped: 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Apparent  Purity. 

SAMPLING 

Take  a  sample  from  the  discharge  of  the  crystallizer  a  few 
minutes  after  the  gate  has  been  opened. 

ANALYSIS 

Follow  the  " General  Methods." 

29.     LOW  GREEN  AND  WASH  SYRUPS. 

Determine   either  once   or   twice  during  the   spinning  of   every 
crystallizer,  or  at  regular  intervals  of  every  2  hours: 
(a)     Apparent  Purity. 

SAMPLING 

Sample  in  the  same  manner  as  "High  Green  and  Wash 
Syrup." 

ANALYSIS 

Follow  the  "General  Methods." 

30.     REMELT   SUGAR 

Determine  every  4  hours: 

(a)  Apparent  Purity. 

(b)  Polarization. 
Determine  every  24  hours: 

(c)  Sulphuric  Acid  (SO,). 

SAMPLING 

A  laboratory  employe  should  take  samples  at  irregular  inter- 
vals, preferably  from  the  discharge  of  the  scroll  into  the  melter, 
or  at  some  other  suitable  place  if  this  is  not  possible.  Keep  in. 


36  METHODS  OF  ANALYSIS 

a  covered  can,  and  mix  thoroughly  before  analysis,  taking  care 
to  break  up  any  lumps.  For  the  sulphuric  acid  determination 
make  up  a  24  hour  composite  sample  by  mixing*  equal  portions  of 
the  samples  prepared  every  4  hours  for  the  regular  laboratory 
analysis. 

ANALYSIS 

(a)  Apparent  Purity:    Weigh  out  130  grams  in  a  counter- 
poised copper  beaker,  dissolve  in  hot  water,  pour  into  a  500  ml 
Kohlrausch  flask,  rinsing  the  beaker  with  water,  cool  to  approxi- 
mately 20°,  make  up  to  the  mark  with  water,  shake  well,  and  deter- 
mine the  apparent  purity  as  in  the  "General  Methods." 

(b)  Polarization:    Increase  the  polariscope  reading  obtained 
in  the  apparent  purity  determination  by  one-tenth  of  its  value. 

(c)  Sulphuric  Acid  (SOJ:    Follow  the  "General  Methods," 
using  20  grams  of  material. 

31.     SUGAR  MELTER 

Determine  every  8  hours: 

(a)  Brix. 

(b)  Apparent  Purity. 

Determine  every  2  hours,  when  lime  is  added  to  the  melter : 

(c)  Alkalinity. 

SAMPLING 

Take  a  catch  sample  from  the  melter  or  melter  pump. 

ANALYSIS 

(a)  Brix  and  (b)  Apparent  Purity:  Follow  the  "General 
Methods."  In  case  lime  is  added  to  the  melter,  the  sample  should 
be  carbonated  and  filtered  before  the  purity  is  determined,  as  in 
the  case  of  "First  Saturation  Juice.'1 

(c)  Alkalinity:  Measure  out  10"  ml  and  titrate  in  the  cold 
with  N/28  sulphuric  acid  according  to  the  "General  Methods." 

32.     MOLASSES  PRODUCED 

Determine  every  8  hours : 
(a)     Brix. 


II.      REGULAR  FACTORY  CONTROL  37 

(b)  Sugar. 

(c)  Apparent  Purity. 

Determine  at  least  every  24  hours: 

(d)  True  Purity. 

(e)  Raffinose  (%  on  dry  substance). 

SAMPLING 

Draw  at  least  one  sample  from  every  scale  tank  weighed,  and 
if  possible  take  several  samples  at  intervals  during  the  period  when 
the  tank  is  being  filled  or  emptied.  Composite  the  individual 
samples  in  a  large  bucket  and  mix  well  before  analysis. 

ANALYSIS 

Follow  the  * '  General  Methods. ' '  Obtain  the  dry  substance  for 
the  true  purity  determination  either  by  the  refractometer  or  by 
oven  drying. 

33.     CONDENSED  WATERS 

Examine  every  hour : 

(a)  Boiler   feed  water    (both   the    "tank"   and    "returned 
direct"),  press  wash  water,  pure  and  impure  battery  supply  water. 

Examine  every  2  hours: 

(b)  All  individual  pan  and  evaporator  tail  pipes. 

SAMPLING 

Collect  continuous  samples  with  an  automatic  sampling  device. 
Protect  the  samples  from  contamination  both  during  the  time  when 
they  are  being  drawn  and  when  they  are  being  brought  to  the 
laboratory. 

See  Chap.  XVII,  2,  regarding  the  collection  of  campaign  sam- 
ples for  analysis,  and  of  weekly  samples  of  battery  supply  water. 

EXAMINATION 

Test  with  alpha-naphthol  as  described  in  the  "General  Meth- 
ords,"  I,  13.  As  the  reagents  employed  frequently  become  con- 
taminated, check  them  up  every  day  with  water  of  negative 
reaction. 


38  METHODS  OF  ANALYSIS 

NOTE:  If  sugar  is  found,  determine  the  source  at  once  and 
report  it  to  the  operating  department.  It  is  desirable  to  have  in 
use  a  "board"  or  some  system  representing  a  flow  chart  of  the 
condensed  waters,  in  order  that  the  source  of  sugar  may  be  readily 
and  quickly  located. 

34.     BOILER  WATER. 

Determine  every  8  hours  on  each  boiler  in  service : 
(a)     Alkalinity. 

SAMPLING 

Draw  from  the  sampling  line,  first  allowing  the  water  to  run 
a  few  moments  to  rinse  out  the  pipe. 

ANALYSIS 

Measure  out  10  ml  with  a  pipette  into  a  porcelain  dish  and 
follow  the  "General  Methods,"  10  (a),  using  phenolphthalein  as 
indicator.  Dilute  with  sufficient  neutral  water  to  make  the  color 
reaction  distinct. 

35.     WEEKLY  COMPOSITE   SAMPLES 

Determine : 

(a)  Brix. 

(b)  Apparent  Purity. 

(c)  Dry  Substance   (by  oven  drying). 

(d)  Sugar  (direct  polarization). 

(e)  Sugar  by  Inversion. 

(f)  Raffinose. 

(g)  Invert  Sugar, 
(h)  Ash  (Sulphated). 
(i)  Undetermined. 

(j)  Lime  Salts  (CaO  to  100  Brix). 

(k)  Sulphuric  Acid  (S03). 

(1)  Organic  Coefficient. 

(m)  Dry  Substance  (by  refractometer,  if  available). 

SAMPLING 

Make  up  an  average  sample  of  each  of  the  following  products 
by  taking  equal  portions  of  each  sample  brought  to  the  laboratory 


II.   REGULAR  FACTORY  CONTROL  39 

during  the  week  and  preserving  in  a  sealed  jar  or  stoppered  bottle. 

(1)  Evaporator  Thick  Juice. 

(2)  White  Massecuite. 

(3)  Remelt  Massecuite  (from  pan). 

(4)  Remelt  Sugar. 

(5)  Molasses  Produced. 

(6)  Molasses  Worked. 

(7)  Cold  Saccharate  Cake. 

(8)  Cold  Perfectly  Washed  Saccharate  Cake. 

(9)  Hot  Saccharate  Cake. 

(10)  Hot  Perfectly  Washed  Saccharate  Cake. 

(11)  Saccharate  Milk. 

In  the  case  of  the  saccharate  cakes  and  milk,  use  the  thick 
syrup  obtained  by  evaporating  the  thin  juice  from  the  apparent 
purity  determination  to  60-70°  Brix  on  a  water  bath.  Concentrate 
this  juice  as  soon  as  it  is  available,  not  allowing  it  to  stand  in  a 
thin  condition.  When  the  massecuite  samples  are  desired  for 
analysis,  heat  the  containers  by  immersion  in  hot  water,  remove 
the  contents,  and  mix  thoroughly  in  order  to  obtain  a  uniform 
mixture  of  sugar  crystals  and  mother  syrup. 

ANALYSIS 

Follow  the  "General  Methods."  Analyses  may  be  made,  if 
desired,  on  "double  diluted"  solutions  in  the  case  of  massecuites, 
raw  sugar,  and  molasses,  using  twice  the  amount  of  material  as 
when  analyzing  original  material  direct.  Preserve  the  double 
diluted  solutions  from  decomposition  with  3  to  4  drops  of  a  40% 
formaldehyde  solution,  but  do  not  use  any  double  diluted  material 
which  has  stood  for  more  than  eight  hours.  Determine  the  dry 
substance  in  Remelt  Sugar  by  heating  approximately  5  grams 
without  dissolving  in  water  and  without  the  use  of  sand. 

Make  all  the  prescribed  determinations  except  as  follows : 

(1)  Omit  the   Brix   determination   in   the   case   of  Remelt 
Sugar. 

(2)  In  the  case  of  the  Cold  and  Hot  Perfectly  Washed  Cakes 
determine  only  the  Brix,  dry  substance,  sugar,  sugar  by  inversion, 
raffinose,  ash,  and  apparent  purity. 

To  obtain  the  "percentage  on  dry  substance"  in  any  case, 
multiply  the  "percentage  on  original"  by  100  and  divide  by  the 
percentage  of  dry  substance.  Use  the  dry  substance  found  by 
oven  drying  in  calculating  percentages  on  dry  substance. 


40  METHODS  OP  ANALYSIS 

To  obtain  (i)  Undetermined,  subtract  from  100  the  sum  of 
the  percentages  of  (e)  Sugar  by  Inversion,  (f)  Eaffinose,  (g) 
Invert  Sugar,  and  (h)  Ash  (all  percentages  on  dry  substance). 

Calculate  (1)  Organic  Coefficient  as  described  in  the  "General 
Methods,"  I,  8. 

NOTE:  See  Chap.  XVII,  2  (b)  regarding  the  collection  of 
weekly  average  samples  of  pure  and  impure  battery  supply  water 
for  the  determination  of  total  solids. 

36.     TEMPERATURE  DATA. 

GENERAL 

Obtain  the  necessary  temperature  data  either  from  the  charts 
of  recording  thermometers  or  by  averaging  readings  taken  every 
2  hours  by  a  laboratory  employe.  Check  recording  thermometers 
previous  to  every  campaign,  and  if  possible  at  occasional  intervals 
during  the  campaign.  It  is  advisable  to  have  provision  for  a  well 
near  each  recording  thermometer,  by  means  of  which  the  latter 
may  be  checked  in  situ  with  an  accurate  indicating  thermometer. 

The  following  directions  apply  to  particular  cases. 

DIFFUSION  BATTERY  TEMPERATURE  READINGS 

A  laboratory  employe  should  take  a  series  of  readings  of  the 
thermometers  on  each  battery,  starting  in  every  case  at  the  "cos- 
sette  cell ' '  and  continuing  successively  along  the  other  cells  in  cir- 
culation. Do  not  record  readings  of  any  cells  not  in  circulation 
at  the  time.  Take  the  readings  at  least  every  2  hours. 

In  order  that  the  figures  obtained  may  be  comparable  at  all 
factories,  observe  also  the  following  precautions : 

(1)  Commence  the  readings  immediately  after  the  period  of 
"sending  over"  begins  and  not  during  the  period  of  diffusing  a 
fresh  cell. 

(2)  The  figure  reported  for  the  temperature  of  cell  No.  1 
should  represent  the  temperature  of  the  juice  entering  the  cossette 
cell  and  not  the  temperature  of  the  juice  from  the  cossette  cell 
which  goes  to  the  measuring  tank. 

(3)  The  last  temperature  reading  should  represent  the  tem- 
perature  of  the  battery   supply   water   entering   the   "pulp"   or 
"water"  cell.     The  arrangement  of  thermometers  on  the  batteries 


II.      REGULAR  FACTORY  CONTROL  41 

is  such  that  in  most  cases  this  reading  can  be  obtained  from  a 
battery  thermometer. 

(4)  As  the  position  of  the  thermometers  on  different  bat- 
teries varies,  the  matter  should  be  gone  over  individually  at  each 
factory  and  arrangements  should  be  made  to  have  the  readings 
properly  taken. 

Obtain  the  "average  maximum  temperature  of  the  battery" 
by  averaging  the  temperature  readings  of  those  cells  carried  at 
the  maximum  temperature. 

JUICE  LEAVING  FIRST  PRESSES 

Obtain  every  2  hours  by  filling  a  sample  bucket  from  the  press 
cocks  and  taking  a  reading  immediately  with  a  mercury  ther- 
mometer. 

SUGAR  LEAVING  UPPER  GRANULATORS 

Fill  a  sample  bucket  every  2  hours  from  the  discharge  from 
the  upper  to  the  lower  granulator  arid  insert  the  bulb  of  a  mercury 
thermometer  into  the  middle  of  the  mass  of  sugar. 

SUGAR  AS  SACKED 

Take  readings  every  2  hours  by  inserting  a  mercury  ther- 
mometer deeply  into  a  bag  of  sugar  just  filled  at  the  sacking 
station. 

REMELT  MASSECUITE  AS  DROPPED 

Insert  a  mercury  thermometer  in  the  sample  taken  for  the 
laboratory  analysis;  obtain  the  reading  immediately  after  the 
sample  is  taken.  Or  obtain  the  information  from  the  pan  recording 
thermometer  or  the  sugar  boiler's  record. 

KKMKLT  M.\ SMECTITE  AS  SPUN 

Take  a  sample  every  2  hours  from  the  goosenecks  of  the  mixer 
and  insert  a  mercury  thermometer. 


HI.  SULPHATE  CONTROL 


1.  INTRODUCTION 

Whenever  the  concentration  of  sulphuric  acid  in  the  remelt 
massecuite  exceeds  the  amount  which  can  be  held  in  solution  and 
eliminated  in  the  molasses  (usually  1.0 — 1.5  per  cent  S03  on  mo- 
lasses dry  substance),  the  excess  crystallizes  out,  mostly  as  potas- 
sium sulphate,  in  the  remelt  sugar.  This  not  only  impairs  the 
quality  of  the  remelt  sugar,  but  may  even  in  extreme  cases  lead 
to  the  presence  of  small  amounts  of  S03  in  the  white  sugar.  The 
usual  practice  to  control  this  is  the  treatment  of  the  melted  sugar, 
when  necessary,  with  barium  oxide,  calcium  chloride,  or  lime.  The 
special  sulphate  control  described  in  this  chapter  is  designed  to 
throw  light  on  the  amount  of  sulphuric  acid  in  the  various  products, 
including  the  amount  formed  in  sulphuring  the  juice,  and  on  the 
efficacy  of  the  melted  sugar  treatment  when  used. 

The  determination  of  sulphuric  acid  (S03)  in  the  remelt  sugar 
(see  section  7)  is  prescribed  as  a  regular  daily  test,  The  deter- 
mination should  be  made  also  in  the  white  sugar  (section  6) 
whenever  the  S03  in  the  remelt  sugar  exceeds  1.00  per  cent.  The 
determinations  described  in  sections  7 — 10  should  be  made  when- 
ever treatment  for  the  removal  of  sulphates  is  being  employed. 
The  determinations  described  in  sections  2 — 6  are  for  use  on  special 
occasions  when  it  is  desired  to  investigate  the  amount  of  sulphuric 
acid  formed  at  the  sulphur  stations. 

2.     SECOND  SATURATION  JUICE 

Determine : 

(a)     Sulphuric  Acid  (S03  to  100  Brix). 


III.      SULPHATE  CONTROL  43 

SAMPLING 

Make  up  a  composite  sample  by  mixing  equal  amounts  of  the 
composite  samples  prepared  every  4  hours  for  the  regular  labora- 
tory analysis.  (See  Chap.  II,  6.)  Use  a  few  drops  of  formalde- 
hyde to  preserve  the  samples. 

ANALYSIS 

(a)  Sulphuric  Acid  (S03  to  100  Brix):  Follow  the  "General 
Methods,"  Chap.  I,  9.  Either  determine  the  Brix  or  use  the 
average  of  the  regular  Brix  determinations. 

3.     THIRD  SATURATION  JUICE 

Determine : 

(a)     Sulphuric  Acid  (S03  to  100  Brix). 

SAMPLING  AND  ANALYSIS 

Make  up  a  composite  sample  and  analyze  in  a  similar  manner 
to  "2.  Second  Saturation  Juice." 

4.  BLOW-UP  THICK  JUICE  BEFORE  SULPHUR 

Determine : 

(a)     Sulphuric  Acid  (S03  to  100  Brix). 

SAMPLING  AND  ANALYSIS 

Make  up  a  composite  sample  from  the  samples  of  evaporator 
thick  juice  prepared  every  4  hours  for  the  regular  laboratory 
analysis,  and  analyze  in  a  similar  manner  to  "2.  Second  Satura- 
tion Juice." 

Note:  If  melted  sugar  is  added  to  the  blow-ups,  this  deter- 
mination is  of  no  value. 

5.  BLOW-UP   THICK   JUICE   AFTER  SULPHUR 

Determine : 

(a)  Brix. 

(b)  Sulphuric  Acid  (S03  to  100  Brix). 


44  METHODS  OF  ANALYSIS 

SAMPLING  AND  ANALYSIS   . 

Make  up  a  composite  sample  from  the  samples  prepared  every 
4  hours  for  the  regular  laboratory  analysis,  and  analyze  in  a  simi- 
lar manner  to  "2.  Second  Saturation  Juice."  Determine  the 
Brix  in  the  regular  manner. 

6.     WHITE  SUGAR 

Determine  every  24  hours : 

(a)     Sulphuric  Acid  (S03  011  original). 

SAMPLING 

Make  up  a  composite  sample  by  mixing  equal  amounts  of 
the  samples  of  Standard  granulated  sugar  prepared  every  8  hours 
for  the  moisture  determination. 

ANALYSIS 

Follow  the  "General  Methods/'  I,  9.  Make  a  blank  S03  test 
on  the  distilled  water  and  reagents,  and  deduct  the  correction 
found  from  the  amount  found  in  the  analysis  of  the  sugar. 

7.     REMELT  SUGAR 

Determine  every  24  hours : 

(a)     Sulphuric  Acid  (S03  on  original). 

SAMPLING 

Make  up  a  composite  sample  by  mixing  equal  portions  of  the 
samples  prepared  every  4  hours  for  the  regular  laboratory  analysis. 

ANALYSIS 

Follow  the  "General  Methods,"  making  sure  that  an  excess 
of  barium  chloride  solution  is  added. 

NOTE:  This  is  a  test  required  in  the  "Regular  Factory  Con- 
trol." See  Chap.  II,  30,  (c). 

8.  MELTED  SUGAR  BEFORE  TREATMENT 

Determine  every  hour: 

(a)     Alkalinity.     (Determine  only  when  lime  or  barium  oxide 
is  used  for  treatment.) 


HI.      SULPHATE  CONTROL  45 

Determine  every  24  hours : 

(b)  Brix. 

(c)  Sulphuric  Acid  (S03  to  100  Brix). 

SAMPLING 

If  lime  or  barium  oxide  is  being  used  for  treatment,  which  is 
usually  continuous,  take  a  catch  sample  from  the'melter  every  hour. 
If  calcium  chloride  is  used  for  treatment,  which  is  usually  inter- 
mittent, take  a  catch  sample  of  each  lot  treated  previous  to  the  addi- 
tion of  the  calcium  chloride.  Make  up  a  composite  sample  by  mix- 
ing equal  portions  of  the  individual  samples. 

ANALYSIS 

(a)  Alkalinity:     If  the  alkalinity  is  0.2  or  less,  titrate  10 
ml  with  N/28  acid  according  to  the  general  method  for  alkalinity. 
If  the  alkalinity  is  higher,  titrate  50  ml  with  Steffen  acid;  in  this 
case  divide  the  number  of  ml  of  acid  used  by  10  to  obtain  the  al- 
kalinity in  terms  of  * '  grams  of  CaO  per  100  ml. ' ' 

(b)  Brix  and  (c)  Sulphuric  Acid  (S03  to  100  Brix):    Fol- 
low the  ' '  General  Methods. ' ' 

9.  MELTED  SUGAR  AFTER  TREATMENT 

Determine  every  8  hours,  as  in  regular  factory  control : 

(a)  Brix. 

(b)  Apparent  Purity. 

Determine  every  24  hours : 

•(c)     Sulphuric  Acid  (S03  to  100  Brix). 

SAMPLING 

Take  a  catch  sample  every  2  hours,  if  possible,  from  the  cocks 
or  trough  of  the  filter  press.  Mix  equal  amounts  of  these  samples 
to  obtain  the  composite  samples  when  needed. 

ANALYSIS 

(a)  Brix  and  (b)  Apparent  Purity:  Follow  the  ''General 
Methods."  In  case  lime  or  barium  oxide  is  added  to  the  melter, 
the  sample  should  be  carbonated  and  filtered  before  the  purity  is 
determined,  as  in  the  case  of  "First  Saturation  Juice."  (See 
Chap.  II,  5.) 


46  METHODS  OF  ANALYSIS 

(c)     Sulphuric  Acid  (S03  to  100  Brix) :    Follow  the  ' '  General 
Methods." 

10.     SULPHATE  CAKE 

Determine  every  24  hours : 

(a)  Sugar. 

(b)  Sulphuric  Acid  (S03). 

SAMPLING 

Follow  in   general  the  method   of  sampling   outlined  under 
"Lime  Cake.,  First  Presses,"  Chap  II,  13. 

ANALYSIS 

(a)  Sugar:     Use  either  of  the  methods  for  "total  sugar" 
described  under  "Lime  Cake,  First  Presses,"  Chap.  II,  13  (a). 

(b)  Sulphuric  Acid  (SOJ:     Weigh  out  2 — 5  grams  of  cake, 
add  100  ml  of  water,  neutralize  with  hydrochloric  acid,  and  add 
3  ml  in  excess.    Boil  for  a  few  minutes,  filter,  and  proceed  as  in 
the  "General  Methods,"  Chap.  I,  9,  making  sure  that  an  excess 
of  barium  chloride  solution  is  added. 


IV.     STEFFEN  PROCESS  CONTROL 


1.     GENERAL 

All  samples  in  connection  with  the  Steffen  Process  control 
must  be  taken  by  a  laboratory  employe. 

2.     MOLASSES  WORKED 

Determine  every  8  hours : 

(a)  Brix. 

(b)  Sugar. 

(c)  Apparent  Purity. 

Determine  every  24  hours: 

(d)  Sugar  by  Inversion  (Per  cent  on  original). 

SAMPLING 

Take  a  catch  sample  at  least  every  2  hours,  and  preferably 
every  hour,  at  the  molasses  scale  tank.  Keep  the  individual  samples 
in  a  covered  container,  and  mix  thoroughly  previous  to  analysis. 

ANALYSIS 

Follow  the  " General  Methods."  Determine  the  direct  polar- 
ization and  the  polarization  after  inversion  on  a  composite  sample 
representing  the  molasses  worked  during  the  entire  24  hours,  and 
calculate  the  percentage  of  "sugar  by  inversion"  in  the  molasses. 


3.     SOLUTION  FOR  COOLER 

Determine  every  3  hours : 
(a)     Brix. 


48  METHODS   OF  ANALYSIS 

(b)  Alkalinity. 

(c)  Sugar  (grams  in  100  ml). 

SAMPLING 

Take  a  catch  sample  of  the  solution  iri  the  cooler  after  the  pro- 
peller has  been  started  and  immediately  preceding  the  beginning 
of  the  lime  addition. 

ANALYSIS 

( a )  Brix :    Follow  the  "  General  Methods. ' ' 

(b)  Alkalinity:    Mix  the  sample  well  and  transfer  50  ml  with 
a  pipette  to  a  100  ml  flask.    Add  a  few  drops  of  phenolphthalein 
and  titrate  to  neutrality  with  Steffen  standard  acid  (1  ml  =  .05 
g  CaO).     Divide  by  10  the  number  of  ml  of  acid  required.     See 
1 '  General  Methods,  "1,10  ( c ) . 

(c)  Sugar:  Add  3 — 6  ml  of  basic  lead  acetate  to  the  neutral- 
ized solution  obtained  in  (b),  fill  to  the  100  ml  mark  with  water, 
shake,  filter,  and  polarize  in  a  200  mm  tube.    Multiply  the  reading 
by  .52  or  use  Table  9,  to  obtain  the  grams  of  sugar  in  100  ml. 

4.     LIME  POWDER 

Determine  every  8  hours : 

(a)  Loss  on  Ignition. 

(b)  CaO  by  Titration. 

(c)  Percentage  Coarser  than  200  mesh. 

SAMPLING 

Take  a  catch  sample  every  hour  from  the  discharge  of  each  mill 
in  operation,  taking  an  equal  amount  of  material  from  each  mill. 
Composite  the  hourly  samples  by  transferring  to  glass  bottles  pro- 
vided with  tightly  fitting  rubber  or  ground  stoppers,  keeping  sepa- 
rate samples  for  each  mill.  For  (a)  Loss  on  Ignition  and  (b)  CaO 
~by  Titration,  make  up  a  composite  sample  by  taking  equal  portions 
from  each  mill  composite  and  mixing  thoroughly. 

ANALYSIS 

(a)  Loss  on  Ignition:  Weigh  out  approximately  1  gram  on 
an  analytical  balance,  in  a  covered  platinum  crucible.  Ignite  to 
constant  weight  in  an  electric  furnace  or  over  a  good  blast  lamp, 


IV.      STEFFEN    PROCESS    CONTROL  49 

cool  in  a  desiccator,  and  weigh.     Multiply  the  loss  in  weight  by 
100  and  divide  by  the  weight  of  the  sample. 

(b)  CaO  by  Tit  rat  ion:     Weigh  out  5  grams,  transfer  to  a 
porcelain  casserole,  and  follow  the  " General  Methods,"  I,  11. 

(c)  Percentage  Coarser  than  200  mesh:    Determine  for  each 
mill  separately.    Weigh  out  20  grams  on  a  pulp  balance,  and  trans- 
fer to  a  200  mesh,  brass  wire  sieve  (width  of  opening  =  .0029  inch) . 
Brush  the  material  carefully  with  a  two-inch  flat  camel  hair  brush 
until  practically  no  more  fine  powder  passes  through.    Weigh  the 
coarse  residue  on  a  pulp  balance.     Multiply  the  weight  of  the 
residue  by  5  to  obtain  the  percentage.     When  the  sieve  becomes 
clogged,  clean  it  with  hydrochloric  acid,  rinse  it  well  with  water, 
and  dry  it  in  a  warm  place. 

SPECIAL  DETERMINATIONS 

(d)  Sugar-soluble  CaO:    Rinse  5  grams  of  lime  powder  into 
a  200  ml  flask,  and  add  150  ml  of  a  freshly  prepared,  25°  Brix 
sugar  solution.      (Or  add  approximately  40  grams  of  sugar  and 
dissolve  by  the  addition  of  water.)     Fill  to  the  mark  with  water, 
stopper  the  flask  and  shake  vigorously,  repeating  the  shaking  at 
short  intervals  as  the  lime  settles  to  the  bottom.    Filter  at  the  end 
of  thirty  minutes,  and  titrate  100  ml  with  the  standard  nitric  acid 
(1  ml  =  .05  g  CaO),  using  phenolphthalein  as  indicator.    Multiply 
by  2  the  number  of  ml  of  acid  required,  to  obtain  the  percentage 
of  CaO. 

(e)  Slacking  Test:..  Into  a  beaker  of  250  ml  capacity  measure 
out  100  ml  of  water  at  exactly  20°.     Add  25  grams  of  the  lime 
powder,  using  a  thermometer  as  a  stirring  rod,  and  continue  to 
stir  until  there  is  no  further  rise  in  temperature.    Record  the  num- 
ber of  degrees  increase  in  temperature  over  the  original  20°,  and 
the  number  of  minutes  required  to  attain  the  maximum  tempera- 
ture. 

5.     COOLER  WASTE  WATER 


Determine  every  hour: 

(a)     Sugar  (grams  in  100  ml). 


SAMPLING 

Take  a  catch  sample,  just  previous  to  the  time  it  is  required  for 
analysis,  from  a  finished  cooler,  after  all  the  lime  has  been  added, 
and  just  before  the  finished  cooler  is  dropped. 


50  METHODS  OP  ANALYSIS 

ANALYSIS 

Filter  a  portion  immediately  through  filter  paper.  Transfer 
50  ml  of  the  filtrate  with  a  pipette  to  a  100  ml  flask,  add  a  few  drops 
of  phenolphthalein,  neutralize  with  Steffen  standard  acid,  and  pro- 
ceed as  in  the  determination  of  sugar  in  "Cold  Press  Waste 
Water,"  6  (c). 

6.     COLD  PRESS  WASTE  WATER 

Determine  every  2  hours: 

(a)  Brix. 

(b)  Alkalinity. 
Determine  every  hour : 

(c)  Sugar  (grams  in  100  ml). 

SAMPLING 

Collect  a  continuous  sample  from  the  cold  waste  water  line 
in  the  manner  described  below  under  "7.  Total  Waste  Water,'"' 
or  take  a  catch  sample  every  hour  from  the  discharge  of  the  cold 
presses.  Mix  the  sample  well  before  analysis. 

ANALYSIS 

(a)  Brix:     Follow  the  "General  Methods." 

(b)  Alkalinity:     Transfer  50  ml  with  a  pipette  to  a  100  ml 
flask.    Add  a  few  drops  of  phenolphthalein  and  titrate  to  neutrality 
with  Steffen  standard  acid  (1  ml  =  .05  g  CaO).    Divide  the  num- 
ber of  ml  of  acid  required  by  10.  See  "General  Methods,"  I,  10  (c). 

(c)  Sugar:  Add  2 — 4  ml  of  basic  lead  acetate  to  the  neutral- 
ized solution  obtained  in  (b),  fill  to  the  100  ml  mark  with  water, 
shake,  filter,  and  polarize  in  a  200  mm  tube.    Multiply  the  reading 
by  .52,  or  use  Table  9,  to  obtain  the  grams  of  sugar  in  100  ml. 

7.     TOTAL  WASTE  WATER 

Determine  every  2  hours: 

(a)  Brix. 

(b)  Alkalinity. 
Determine  every  hour: 

(c)  Sugar  (grams  in  100  ml). 


IV.      STEPFEN   PROCESS    CONTROL  51 

SAMPLING 

Collect  an  average  sample  from  the  pipe  line  which  conducts 
the  final  waste  water  outside  the  factory,  by  means  of  a  continuous, 
automatic  sampling  device  which  delivers  into  a  large  vessel  pro- 
vided with  an  overflow  at  the  top  and  a  drain  at  the  bottom.  Mix 
the  entire  sample,  take  a  small  portion  for  analysis,  and  empty 
c»ut  the  remainder  by  opening  the  drain  valve. 

If  for  any  reason  it  is  impossible  to  secure  a  continuous  sample, 
take  a  catch  sample  every  hour.  Mix  the  sample  well  before  analysis. 

ANALYSIS 

Analyze  as  in  the  case  of  "Cold  Press  Waste  Water,"  cooling 
first  if  necessary. 

8.     COLD  WASH  WATER  (FINAL) 

Determine  every  4  hours : 
(a)     Brix. 

SAMPLING 

Sample  the  wash  water  coming  from  the  presses  at  the  time 
when  the  washing  is  finished.  The  sample  used  for  analysis  should 
preferably  represent  a  composite  of  samples  obtained  from  at  least 
three  presses.  This  sample  cannot  be  obtained  at  factories  equipped 
with  vacuum  filters. 

ANALYSIS 

Determine  the  Brix  in  the  regular  manner. 

9.     COLD  WASH  WATER  (AVERAGE) 

Determine  every  4  hours : 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Sugar  (grams  in  100  ml). 

SAMPLING 

Take  a  sample  from  the  wash  water  tank. 

ANALYSIS 

Analyze  as  in  the  case  of  ' '  Cold  Press  Waste  Water. ' ' 


52  METHODS  OF  ANALYSIS 

10.     HOT  WASH  WATER  (FINAL) 

Determine  every  4  hours : 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Sugar  (grams  in  100  ml). 

SAMPLING 

Sample  in  the  same  manner  as  the  final  cold  wash  water.  The 
sample  must  represent  the  wash  water  coming  from  the  hot  presses 
at  the  time  when  the  washing  is  finished.  At  factories  equipped 
with  vacuum  filters,  where  this  sample  cannot  be  obtained,  substi- 
tute the  "average"  hot  wash  water. 

ANALYSIS 

Analyze  as  in  the  case  of  "Cold  Press  Waste  Water." 

11.     COLD  SACCHARATE  CAKE 

Determine  every  3  hours : 

(a)  Apparent  Purity. 

(b)  Lime  Salts  (CaO  to  100  Brix). 
Determine  every  8  hours : 

(c)  Apparent  Purity  (Perfectly  Washed). 

(d)  Sugar. 

(e)  CaO. 

(f)  CaO  to  100  Sugar. 
Determine  every  24  hours : 

(g)  Moisture. 
(h)     True  Purity. 

(i)     Raffinose  (Per  cent  on  dry  substance), 
(j)     True  Purity  (Perfectly  Washed). 

SAMPLING 

Take  a  sample  once  an  hour  from  various  parts  of  the  cake 
in  several  frames,  using  a  spoon  and  bucket.  In  the  case  of  vacuum 
filters  take  small  portions  of  the  material  dropping  from  the  drums 
of  all  the  units  in  operation.  Sample  Kelly  Presses  in  the  manner 
described  under  II,  13,  "Lime  Cake  Sampling  (Kelly  Presses)." 


IV.      STEFFEN    PROCESS    CONTROL  53 

Preserve  the  samples  in  a  covered  container  and  make  up  com 
posite  samples  at  the  times  when  the  various  determinations  are 
due,  except  as  otherwise  noted.  Mix  all  composite  samples  well. 

ANALYSIS 

(a)  Apparent  Purity:     The  following  special  apparatus  is 
needed:  A  carbonator  with  steam  and  carbon  dioxide  gas  connec- 
tions, and  an  evaporator  heated  by  steam,  both  so  constructed  as 
to  obviate  any  possibility  of  burning  the  juice. 

Mix  a  suitable  amount  of  the  cake  with  4 — 5  parts  of  water  un- 
til a  homogeneous  mixture  is  obtained.  Transfer  to  the  laboratory 
carbonator,  heat  to  80 — 85°,  and  carbonate  at  this  temperature  to 
faint  alkalinity  with  phenolphthalein.  Do  not  carbonate  to  neu- 
trality or  acidity.  When  the  carbonation  is  finished,  heat  to  boiling, 
and  filter.  Concentrate  sufficient  of  the  filtrate  to  about  23°  Brix 
in  the  laboratory  evaporator,  being  careful  not  to  carry  the  evap- 
oration much  beyond  this  point  on  account  of  the  danger  of  burning 
the  juice.  Draw  off  the  liquid  into  a  copper  can  or  suitable  ves- 
sel, and  carbonate  again  to  faint  alkalinity.  Filter,  preferably 
under  vacuum  through  a  Buechner  funnel.  Cool  the  filtrate  in  a 
cylinder  and  determine  the  apparent  purity  as  described  in  the 
''General  Methods." 

(b)  Lime  Salts  (CaO  to  100  Brix):    Use  10  ml  of  the  solu- 
tion prepared  for  the  apparent  purity  determination,  and  follow 
the  "General  Methods,"  12  (a). 

(c)  Apparent  Purity  (Perfectly  Washed) — Apparatus:   Use 
the  regular  equipment  which  consists  of  a  closed  cylindrical  reser- 
voir, a  small  filter  press,  a  vacuum  leaf  filter,  and  a  rectangular 
tank  divided  into  two  sections,  each  of  which  is  subdivided  into 
two  compartments  by  partitions  extending  nearly  to  the  bottom. 
The  reservoir  has  the  necessary  fittings  at  the  bottom  for  connect- 
ing it  to  the  small  press  or  the  vacuum  leaf.     Vacuum,  air  pres- 
sure, charging  lines,  and  a  relief  valve  are  provided  at  the  top  of 
the  tank.     Clean  the  filter  cloths   frequently  with   hydrochloric 
acid  and  water. 

Use  whichever  of  the  following  methods  is  found  to  give  the 
most  consistent  results: 

Method  I  (Elutriation):  Add  3  parts  of  the  coldest  water  ob- 
tainable to  1  part  of  the  sample,  and  stir  until  all  lumps  are  broken 
up  and  a  perfectly  homogeneous  mixture  is  obtained.  Filter  im- 
mediately through  the  laboratory  press,  allowing  the  pressure  to 


54  METHODS  OP  ANALYSIS 

rise  gradually  to  40  pounds  per  square  inch  and  maintaining  this 
pressure  until  the  nitrate  ceases  to  flow  or  comes  in  slow  drops. 
Mix  the  cake  thus  obtained  with  4 — 5  parts  of  water;  and  proceed 
exactly  as  under  (a)  "Apparent  Purity." 

Method  11  (Vacuum  Filtration):  Fill  one  section  of  the  rec- 
tangular tank  of  the  equipment  described  above  with  finished 
cooler  solution  and  submerge  the  leaf  in  one  of  the  compartments. 
Open  the  valves  in  the  vacuum  line  at  the  top  of  the  reservoir  and 
in  the  line  connecting  the  leaf  to  the  bottom  of  the  reservoir,  keep- 
ing all  other  valves  closed.  Maintain  a  vacuum  of  at  least  15  inches 
on  the  gage  and  allow  the  cake  to  form  until  it  is  flush  with  the 
guide,  stirring  the  solution  continually  during  filtration  in  order 
to  insure  the  formation  of  an  even  cake.  When  cake  of  the  re- 
quired thickness  has  formed,  transfer  the  leaf  to  the  other  section 
of  the  tank  which  has  been  filled  with  cold  water,  and  allow  8  liters 
of  wash  water  to  pass  through  the  cake ;  this  is  most  easily  meas- 
ured by  observing  the  level  of  the  water  at  the  time  when  washing 
is  commenced  and  gradually  adding  8  liters  of  cold  water.  When 
the  same  level  is  reached  after  the  addition  of  the  8  liters,  remove 
the  leaf  from  the  tank  and  allow  the  cake  to  dry  for  5  minutes  with 
the  vacuum  on.  Shut  off  the  vacuum,  remove  the  cake,  mix  it  with 
4 — 5  parts  of  water,  and  proceed  exactly  as  under  (a)  "Apparent 
Purity."  If  the  cake  cracks  before  the  washing  is  completed,  dis- 
card it  and  repeat  the  test.  Clean  the  leaf  frequently  by  washing 
it  first  with  hydrochloric  acid  and  then  with  water. 

Method  111  (Combined  Elutriation  and  Washing) :  Take  a 
catch  sample  of  finished  cooler  solution  (about  10  liters  is  required) , 
and  filter  it  immediately  through  the  3%  inch  frame  of  the  labora- 
tory filter  press  under  30  pounds  air  pressure;  do  not  allow  air 
to  go  through  the  cake  by  permitting  the  reservoir  to  run  empty. 
This  will  produce  a  cake  weighing  5%  pounds.  Mix  this  cake  thor- 
oughly and  quickly  with  100%  of  cold  water,  5%  pounds  or  2600 
ml,  and  filter  through  the  2%-inch  frame  of  the  small  press  at  30 
pounds  pressure ;  again,  do  not  allow  air  to  pass  through  the  cake. 
This  will  produce  a  cake  weighing  4%  pounds.  Drain  and  wash  out 
the  reservoir,  then  introduce  100%  of  cold  water,  4%  pounds  or 
2150  ml,  and  force  it  through  the  cake  at  15  pounds  pressure,  al- 
lowing air  to  pass  through  the  cake  for  one-half  minute  after  the 
water  has  all  gone  through.  This  yields  a  final  eake  of  uniform 
weight  and  moisture  content.  Mix  this  cake  with  4 — 5  parts  of 


*It  will  facilitate  the  washing  if  the  plug  at  the  top  of  the  2V2  inch 
frame  is  removed  and  a  small  rod  is  forced  through  the  cake  to  the  port. 


IV.      STEFFEN   PROCESS    CONTROL  55 

water,  and  proceed  exactly  as  under  (a)  "Apparent  Purity."  If 
the  two  frames  used  are  not  of  exactly  the  dimensions  given,  obtain 
a  sufficient  number  of  weights  of  cake  to  establish  the  amount  of 
water  required  for  elutriation  and  washing,  which  should  be  100% 
on  the  weight  of  the  cake  in  each  case. 

(d)  Sugar:    Weigh  oat  13  grams  of  the  cake  in  a  counter- 
poised nickel  dish,  reduce  to  a  thin  cream  with  water,  and  rinse 
into  a  100  ml  flask.    Add  a  few  drops  of  phenolphthalein  and  neu- 
tralize with  dilute  acetic  acid,  avoiding  any  great  excess.    Cool,  add 
3 — 5  ml  of  lead  acetate,  fill  to  the  mark  with  water,  shake,  filter  and 
polarize  in  a  200  mm  tube.     Multiply  the  polariscope  reading  by 
2  to  obtain  the  percentage  of  sugar. 

(e)  CaO:    Weigh  out  10  grams  of  the  cake,  transfer  to  a 
porcelain   casserole,    and   follow   the   "General  Methods,"    I,    11. 
Subtract  the  number  of  ml  of  alkali  from  the  number  of  ml  of 
acid  used,  and  divide  by  2  to  obtain  the  percentage  of  CaO. 

(f)  CaO  to  100  Sugar:    Multiply  the  percentage  of  CaO  by 
100  and  divide  by  the  percentage  of  sugar. 

(g)  Moisture:     Weigh  out  approximately  10  grams  of  the 
composite  cake  sample  in  a  covered  aluminum  dish,  and  dry  for 
5 — 6  hours  at  100 — 105°  as  under  the  determination  of  dry  sub- 
stance in  the  "General  Methods,"  repeating  the  drying  for  one 
hour  periods  until  the  loss  in  any  period  is  not  over  0.2%. 

(h)  True  Purity:  Evaporate  on  a  water  bath  to  approxi- 
mately 50°  Brix  a  sample  composed  of  equal  portions  of  the  23° 
Brix  juice  used  for  the  apparent  purity  determinations.  Deter- 
mine the  true  purity  as  in  the  "General  Methods."  Obtain  the 
dry  substance  either  by  the  refractometer  or  by  oven  drying. 

(i)  Raffinose  (Per  cent  on  dry  substance):  This  is  obtained 
in  connection  with  the  true  purity  determination. 

(j)  True  Purity  (Perfectly  Washed):  Make  up  a  composite 
sample  and  determine  as  under  (h),  using  equal  portions  of  the  23° 
Brix  juice  prepared  for  the  determination  of  the  apparent  purity 
of  the  perfectly  washed  cakes. 

12.     HOT  SACCHARATE  CAKE 

Determine  every  8  hours: 

(a)  Apparent  Purity. 

(b)  Lime  Salts  (CaO  to  100  Brix). 

(c)  Apparent  Purity  (Perfectly  Washed). 


56  METHODS  OF  ANALYSIS 

(d)  Sugar. 

(e)  CaO. 

(f)  CaO  to  100  Sugar. 
Determine  every  24  hours : 

(g)  Moisture 
(h)     True  Purity. 

(i)      Baffin ose  (%  on  dry  substance), 
(j)     True  Purity  (Perfectly  Washed). 

SAMPLING 

Follow  the  methods  described  under  "11.  Cold  Saccharate 
Cake."  In  the  case  of  Vallez  presses,  obtain  the  sample  from  the 
discharge  of  the  press  scroll  before  the  water  is  turned  on.  If 
two  different  kinds  of  filters  are  in  use,  adjust  the  system  of 
sampling  so  as  to  show  the  relative  efficiency  of  the  two  types. 

ANALYSIS 

Follow  the  methods  under  "11.  Cold  Saccharate  Cake."  In 
making  the  perfectly  washed  cake,  use  Method  I  with  the  follow- 
ing modifications  and  precautions:  (1)  Use  a  catch  sample  of  the 
hot  saccharate  cake,  not  allowing  it  to  cool  any  more  than  can  be 
avoided;  (2)  Elutriate  with  hot  water  (nearly  boil'ing)  ;  (3)  Heat 
up  the  apparatus  with  hot  water  before  starting  the  filtration, 

13".     S AC CH ABATE  MILK 


Determine  every  hour: 

(a)  Brix. 

(b)  CaO  (grams  in  100  ml). 
Determine  every  4  hours: 

(c)  Apparent  Purity. 


SAMPLING 

Take  a  catch  sample  from  the  discharge  line  of  the  pump. 
For  the  purity  determination  make  up  a  composite  sample  from 
equal  amounts  of  the  four  previous  hourly  samples. 

ANALYSIS 

(a)  Brix  and  (b)  CaO:  Determine  as  in  the  case  of  "Milk 
of  Lime,"  Chap.  II,  12. 


IV.   STEFFEN  PROCESS  CONTROL  57 

(c)  Apparent  rurity:  To  a  composite  of  the  previous  hourly 
samples  add  3 — 4  parts  of  water,  mix  well,  and  proceed  with  the 
carbonation,  etc.,  as  under  11  (a),  "Cold  Saccharate  Cake- 
Apparent  Purity." 

14.    SMALL  COOLER  TESTS 

Make  occasional  tests  with  the  laboratory  cooler  to  check  up 
the  efficiency  of  the  factory  coolers.  See  Chap.  XXIII,  5  and  17, 
for  directions  regarding  the  speed  and  operation  of  the  cooler. 

Determine : 

(a)  Sugar  in  "Solution  for  Cooler." 

(b)  Lime  Added  to  100  Sugar. 

(c)  Sugar  in  Waste  Water. 

(d)  Percentage  of  Sugar  Precipitated. 

Record  also  the  temperature  at  start  and  finish,   and  the  time 
required  to  add  the  lime. 

SAMPLING 

Use  a  sample  of  molasses  and  dilute  with  water  to  the  required 
density  or  take  a  sample  of  the  "Solution  for  Cooler"  from  the 
factory  coolers.  Take  also  a  sample  of  the  lime  powder  being  used 
in  the  Steffen  House  at  the  time. 

OPERATION  OF  COOLER  TEST 

See  that  the  cooler  is  clean  and  well  drained,  and  pour  in 
14,050  ml  of  the  molasses  solution.  Commence  the  circulation  of 
the  cooling  water.  Allow  the  solution  in  the  cooler  to  come  to  per- 
fect rest,  in  order  to  prevent  the  formation  of  foam  when  the 
propeller  is  started,  then  start  the  propeller,  and,  when  the  solu- 
tion has  become  well  mixed,  remove  50  ml  for  the  determination 
of  the  sugar  content,  leaving  a  volume  of  14,000  ml  of  solution  in 
the  cooler. 

When  the  solution  is  sufficiently  cold,  place  in  the  hopper  the 
weighed  amount  of  lime  which  is  estimated  to  be  sufficient,  or  a 
little  less  than  this  amount,  and  introduce  it  into  the  solution 
through  the  bolter.  When  the  lime  has  all  been  added,  remove  a 
small  amount  of  the  finished  cooler  solution  without  stopping  the 
propeller,  filter  it  immediately,  and  determine  the  sugar  in  the 
regular  mamn'r.  using  50  ml  of  the  filtrate.  If  the  result  shows 


58  METHODS  OF  ANALYSIS 

the  lime  addition  to  be  insufficient,  estimate  the  additional  amount 
required,  add  this,  test  the  finished  cooler  solution  again  as  before, 
and  repeat  this  procedure  until  the  sugar4  in  the  waste  water  is 
reduced  to  the  desired  percentage.  Wash  out  the  cooler  thoroughly 
immediately  after  each  test  to  prevent  the  tubes  from  becoming 
stopped  up,  being  careful  to  avoid  wetting  the  bolter. 

In  general  follow  the  current  factory  practice  with  regard 
to  such  conditions  as  the  temperature  of  precipitation,  the  concen- 
tration of  the  cooler  solution,  and  the  sugar  content  of  the  waste 
water.  It  may  often  be  desirable,  however,  to  vary  some  of  these 
conditions  to  obtain  special  information.  The  time  of  adding  the 
lime  may  also  be  varied  by  changing  the  speed  of  the  conveyor, 
or  by  feeding  the  lime  to  the  conveyor  by  hand,  and  it  will  often 
be  found  that  the  rate  of  adding  the  lime  has  a  great  influence  on 
the  efficiency  of  the  precipitation. 

ANALYSIS 

Use  the  regular  methods  given  elsewhere  in  this  chapter.  Cal- 
culate the  percentage  of  sugar  precipitated  as  follows : 

Let  a  =  sugar  (grams  in  100  ml)  in  Solution  for  Cooler 
b  =  sugar  (grams  in  100  ml)  in  Waste  Water 
x  =  percentage  of  sugar  precipitated 

100  (a  — b) 

Then  x= - - 

a 

Calculate  the  lime  addition  as  follows: 

Let  c  =  grams  of  lime  powder  used 

d  =  volume  of  cooler  solution  in  milliliters  (14000) 
y  =  lime  to  100  sugar 

Then  y==.0001ad 

If,  however,  the  sample  of  " solution  for  cooler"  has  been  obtained 
from  the  factory  coolers  and  therefore  contains  lime  from  the 
previous  cooler,  determine  the  alkalinity  and  correct  the  lime  addi- 
tion as  indicated  in  the  following  formula : 

Let  e  =  alkalinity  (grams  of  CaO  in  100  ml)  of  Solution  for 

Cooler 
f  =  %  CaO  in  lime  powder 

de 

c+  — 
Then  y  = 


.0001  ad 


IV.      STEFFEN   PROCESS    CONTROL  59 

EXAMPLE 

Leta=  5.41 

b  =  .52 

c=  765 
d  =  14000 
e=  .70 

f  =       94.5 

100  (5.41  — .52) 
Then  x  =  _      - :  =  90.4 


765  + 


5.41 
.70  X  14000 


94.5  = 

=  .0001  X  5.41  X  14000 


15.     TEMPERATURE  DATA 

GENERAL 

Refer  to  the  general  instructions  in  the  section  of  the  same 
title  in  Chapter  II,  36.  The  following  directions  apply  to  particular 

a  in  the  Steffen  Process  Control. 

COOLER  SOLUTION,  AVERAGE  MAXIMUM  TEMPERATURE 

Record  the  maximum  temperature  reached  in  each  case  during 
the  cycle  of  a  sufficient  number  of  coolers  to  give  a  fair  average, 
and  derive  the  average  of  these  figures.  Obtain  the  data  from  a 
recording  thermometer  or  from  the  cooler  man's  record. 

(  'OLD  WASTE  WATER,  AVERAGE  TEMPERATURE 

Obtain  every  2  hours  by  filling  a  sample  bucket  from  the  dis- 
charge of  the  cold  presses  and  taking  a  reading  immediately  with 
a  mercury  thermometer.  Or  obtain  from  a  thermometer  installed 
in  the  line  leading  from  the  cold  presses  to  the  heating  system. 

HOT  SOLUTION 

This  should  represent  the  temperature  at  which  the  heated 
waste  water  leaves  the  heating  system  and  should  be  obtained  from 
a  thermometer  suitably  installed  to  indicate  this. 

HOT  WASTE  WATER 

Obtain  every  2  hours  by  filling  a  sample  bucket  from  the  dis- 
charge of  the  hot  presses  and  taking  a  reading  immediately  with 
a.  mercury  thermometer. 


60  METHODS  OF  ANALYSIS 

ADDITIONAL  TESTS  REQUIRED  IN  CONNECTION  WITH 

DORR  THICKENER— VACUUM  FILTER 

INSTALLATIONS 

16.     FEED  TO  THICKENER 

Determine  eveiy  2  hours: 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Sugar  (grams  in  100  ml). 

SAMPLING 

Take  a  catch  sample  every  2  hours  from  the  hot  solution  feed 
line  to  the  Dorr  Thickener,  and  filter  immediately  through  paper. 

ANALYSIS 

Cool  and  analyze  the  filtrate  as  in  the  case  of  "6.  Cold  Press 
Waste  Water." 

17.     OVERFLOW  FROM  THICKENER 

Determine  every  2  hours : 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Sugar  (grams  in  100  ml). 

SAMPLING 

Take  a  catch  sample  every  2  hours,  consisting  of  an  equal 
amount  from  each  of  the  pipe  lines  leading  from  the  overflow 
boxes  to  the  heat  exchanger. 

ANALYSIS 

Mix  the  sample,  cool?  and  analyze  as  in  the  case  of  "Cold  Press 
Waste  Water." 

18.     DISCHARGE  FROM  THICKENER. 

Determine  every  4  hours : 
(a)     Brix. 


IV.      STEFFEN    PROCESS    CONTROL  61 


SAMPLING 


Take  a  catch  sample  of  the  thickened  discharge  every  4  hours, 
<•« insisting  of  an  equal  amount  from  each  of  the  discharges  into  the 
hot  filter  tanks. 

ANALYSIS 

Mix  the  sample  well,  and  transfer  to  a  hydrometer  jar.  After 
cooling  to  approximately  20°,  mix  again  and  determine  the  Brix  in 
the  regular  manner,  taking  the  reading  as  quickly  as  possible 
before  the  suspended  matter  has  time  to  settle. 

19.     HOT  FILTER  WASTE  WATER 

Determine  every  2  hours : 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Sugar  (grains  in  100  ml). 

SAMPLING 

Take  a  catch  sample  every  2  hours  from  the  discharge  into 
the  heat  exchanger. 

ANALYSIS 

Cool  and  analyze  as  in  the  case  of  "Cold  Press  Waste  Water." 


V,     PULP  DRYER  CONTROL 

1.     GENERAL. 

All  samples  in  connection  with  the  Pulp  Dryer  Control  must 
be  taken  by  a  laboratory  employe. 

On  account  of  the  large  number  of  moisture  determinations 
it  is  advisable  to  have  two  drying  ovens.  A  vacuum  oven  is  recom- 
mended for  the  determination  of  moisture  in  "Pulp  Leaving 
Dryer"  and  "Pulp  as  Sacked,"  and  a  double  walled  glycerin 
drying  oven  for  the  other  moisture  and  dry  substance  determina- 
tions; the  temperature  should  be  carried  at  100 — 105°  C.  in  both 
kinds  of  ovens.  Aluminum  dishes,  3  inches  in  diameter  x  %  inch 
high,  provided  with  covers  of  the  same  material,  should  be  used. 

As  the  determination  of  moisture  in  dried  pulp  requires  sev- 
eral hours,  a  rapid'  method  is  employed  to  give  the  operating  men 
better  control.  This  method  is  to  heat  for  1  hour  in  the  oven  and 
multiply  the  loss  found  by  a  factor,  which  is  calculated  from  de- 
terminations made  in  the  regular  manner  by  heating  for  5 — 6  hours 
and  then  for  successive  periods  of  one  hour  until  the  loss  of  weight 
in  one  hour  is  not  over  0.1%.  This  factor  varies  from  1.05  to  1.15, 
and  it  is  recommended  that  a  factor  of  1.10  be  used  until  a  more 
accurate  factor  is  found  for  each  laboratory. 

2.     MOLASSES  TO  PULP  DRYER 

Determine  every  8  hours : 
(a)     Brix. 

SAMPLING 

Take  a  sample  every  2  hours  from  the  molasses  scale  tank  in 
the  Dryer  House.  Transfer  the  individual  samples  to  a  covered 


V.      PULP  DRYER  CONTROL  63 

container  and  mix  thoroughly  previous  to  analysis.     Do  not  take 
any  samples  if  molasses  is  not  being-  used. 

ANALYSIS 

Follow  the  "General  Methods,"  I,  1   (b). 

3.     WATER  FROM  PRESSES 

Determine  every  4  hours : 

(a)  Sugar. 
Determine  every  8  hours : 

(b)  Dry  Substance  (grams  in  100  ml). 

SAMPLING 

Take  a  catch  sample  of  the  water  leaving  the  presses,  being 
careful  not  to  include  water  from  any  other  source  in  the  sample, 
and  analyze  immediately. 

ANALYSIS 

(a)  Sugar:    Determine  as  under  "Pulp  and  Pulp  "Water," 
Chapter  II,  3. 

(b)  Dry  Substance:    Mix  the  sample  well  and  transfer  50  ml 
to  a  weighed  porcelain  evaporating  dish,  being  careful  to  include 
a  proper  proportion  of  the  suspended  matter.     Evaporate  to  dry- 
ness  on  a  water  bath  and  complete  the  drying  in  an  oven  at  100 — 
105° ;  about  11/2  hours  in  the  oven  is  required.    Multiply  the  weight 
of  dry  substance  by  2  to  obtain  the  percentage. 

4.     WATER  FROM  PULPEFANGER 

Determine  every  8  hours: 

(a)     Dry  Substance  (grams  in  100  ml). 

SAMPLING 

Take  a  catch  sample  of  the  water  leaving  the  pulpef  anger,  and 
analyze  immediately. 

ANALYSIS 

(a)  Dry  Substance:  Mix  the  sample  and  determine  as  under 
•'Water  from  Presses." 

Note:  Special  tests  on  this  and  other  waters,  to  determine  the 
amount  of  fine  particles  of  pulp  in  suspension,  may  be  made  as  follows: 


64  METHODS  OF  ANALYSIS 

Determine  the  dry  substance  after  nitration  through  paper;  the  difference 
between  this  and  the  total  amount  of  dry  substance  will  show  the  maxi- 
mum amount  that  can  be  removed.  Determine  the  dry  substance  also 
after  pouring  the  water  through  a  sieve  having  the  same  width  of  open- 
ing as  the  pulpef anger  screen;  this  will  give  an  approximate  idea  of  the 
amount  that  it  is  possible  to  recover  under  working  conditions. 

5.     PULP  ENTERING  PRESSES 

Determine  every  8  hours : 
(a)     Moisture. 

SAMPLING 

Take  a  good-sized  sample  (several  quarts)  from  the  discharge 
of  the  separator,  in  such  a  manner  as  to  secure  as  representative 
a  sample  as  possible  of  the  material  discharged,  using  a  dipper 
which  will  catch  all  of  the  accompanying  water  as  well  as  the  actual 
pulp.  If  it  is  impossible  to  obtain  the  sample  at  this  place,,  take 
the  sample  from  the  slide  to  the  presses,  sampling  from  at  least  two 
presses  which  are  running  and  using  care  to  get  an  average  sample. 

Put  the  entire  sample  in  a  "pulp  can"  of  the  same  type  used 
for  the  samples  of  pulp  from  the  diffusion  battery,  and  after  al- 
lowing it  to  drain  for  15  minutes,  or  longer,  weigh  separately  the 
drained  pulp  and  water  thus  obtained.  (The  water  may  be  meas- 
ured instead  of  weighed,  if  desired. )  Grind  the  drained  pulp  in  an 
Enterprise  Meat  Chopper  and  mix  it  well.  Save  portions  of  the 
pulp  and  the  water  for  analysis. 

ANALYSIS 

Weigh  out  10  grams  of  the  ground  pulp  in  a  3x%-inch  alumi- 
num dish,  and  dry  at  100 — 105°  in  a  glycerin  oven  for  6 — 8  hours, 
or  for  a  period  which  has  been  found  to  be  long  enough  to  give  con- 
stant weight.  In  establishing  this  period  consider  the  weight  con- 
stant when  the  loss  after  an  additional  heating  for  one  hour  is  not 
over  0.1%.  Check  the  accuracy  of  this  period  at  least  once  a  week. 

Evaporate  50  ml  of  the  drained  water  and  determine  the  dry 
substance  as  under  " Water  from  Presses." 

Calculate  the  percentage  of  moisture  in  the  "pulp  entering 
presses "  as  a  weighted  average  from  the  weights  and  moisture  con- 
tent of  the  drained  pulp  and  water.  E.  g.,  if  4,000  grams  of  drained 
pulp  and  1,000  grams  of  drained  water  are  obtained  containing 
respectively  94.80  and  99.70%  moisture,  the  result  is 
(4000  X  94.80)  +  (1000  X  99.70) 


4000  +  1000 


95.8% 


V.      PULP  DRYER  CONTROL  65 

6.     PULP  LEAVING  PRESSES 

Determine  every  4  hours: 
(a)     Moisture. 

SAMPLING 

Take  a  sample  every  hour  from  the  discharge  of  the  pulp  con- 
veyor, if  it  is  possible  to  secure  the  sample  at  this  point  without 
danger.  Otherwise  take  the  sample  from  the  discharge  spouts  of 
the  presses,  but  distribute  the  sampling  well  among  all  the  presses 
in  operation.  Make  up  a  composite  sample  every  4  hours  and  mix 
it  well. 

ANALYSIS 

(a)  Moisture:  Weigh  out  10  grams  in  a  3x%-inch  aluminum 
dish,  and  dry  at  100 — 105°  in  a  glycerin  oven  for  6 — 8  hours,  or  for 
a  period  which  has  been  found  to  be  long  enough  to  give  constant 
weight.  In  establishing  this  period  consider  the  weight  constant 
when  the  loss  after  an  additional  heating  for  one  hour  is  not  over 
0.1%.  Check  the  accuracy  of  this  period  at  least  once  a  week. 

7.     DRIED  PULP  LEAVING  DRYERS 

Determine  every  3  hours  for  each  drum  separately : 
(a)     Moisture. 

SAMPLING 

Take  representative  catch  samples  from  the  discharge  of  each 
drum  and  analyze  immediately. 

ANALYSIS 

(a)  Moisture:  "Weigh  out  10  grams  in  a  3x%-inch  aluminum 
dish  and  dry  in  a  vacuum  oven  at  100 — 105°  for  exactly  1  hour. 
Cool  in  a  desiccator  and  weigh.  Multiply  the  percentage  loss  by  the 
factor  which  has  been  established,  and  report  as  the  percentage  of 
moisture.  To  control  the  factor  make  frequent  tests  by  heating 
samples  for  2  or  3  hours  longer,  and  then  for  successive  periods  of 
one  hour  until  the  loss  of  weight  in  one  hour  is  not  over  0.1%.  At 
the  beginning  of  the  campaign  use  a  factor  of  1.10  until  a  more  ac- 
curate figure  is  established. 


66  METHODS  OF  ANALYSIS 

8.     DRIED  PULP  AS  SACKED 

Determine  every  3  hours: 

(a)  Moisture. 

(b)  Polarization. 

SAMPLING 

Take  a  sample  every  hour  from  at  least  three  bags  as  they  are 
filled  at  the  sacking  station,  and  keep  in  a  tight  container.  Mix 
the  hourly  samples  to  make  composite  samples  when  needed.  If 
plain  and  molasses  pulp  are  produced  on  the  same  day,  save  samples 
of  each  and  analyze  separately.  Save  portions  of  each  composite 
sample  for  a  weekly  composite  sample.  ( See  ' '  Weekly  Analysis  of 
Dried  Pulp,  "below.) 

ANALYSIS 

(a)  Moisture:    Weigh  out  10  grams  of  the  mixed  composite 
sample  and  dry  for  3 — 4  hours  in  a  vacuum  oven  at  100 — 105°. 
Cool  in  a  desiccator  and  weigh.    Report  the  percentage  loss  at  the 
percentage  of  moisture.    As  the  time  of  drying  necessary  to  elim- 
inate all  the  moisture  varies  considerably,  the  length  of  the  drying 
period  should  be  frequently  checked  and  regulated  accordingly. 

(b)  Polarization:     Weigh   out   *12.6   grams,    transfer   to   a 
200.6  ml  flask,  add  12—15  ml  of  basic  lead  acetate,  and  fill  about 
three-fourths  full  with  water.     Digest  exactly  as  in  the  determina- 
tion of  sugar  in  cossettes,  Chapter  II,  1   (a).     Polarize  in  a  400 
mm  tube  and  multiply  the  reading  by  two  to  obtain  the  percentage 
of  sugar. 

9.     WEEKLY  ANALYSIS  OF  DRIED  PULP 

Make  a  weekly  analysis  of  plain  and  molasses  pulp  separately, 
comprising  the  following  determinations : 

(a)  Moisture. 

(b)  Crude  Protein. 

(c)  Crude  Fat. 

(d)  Crude  Fiber. 


*This  weight  is  figured  as  the  equivalent  of  the  half-normal  weight 
after  allowing  7  ml  as  the  volume  of  the  marc  in  13  grams  of  Molasses 
Pulp  containing  15  per  cent  sugar.  Plain  Pulp  is  so  low  in  polarization 
that  the  same  weight  may  be  used  without  appreciable  error. 


V.      PULP   DRYER   CONTROL  67 

(e)  Ash. 

(f)  Nitrogen-free  Extract. 

SAMPLING 

Save  15  grams  of  each  sample  used  for  the  analysis  of  "  Dried 
Pulp  as  Sacked,"  and  keep  in  a  tight  container.  Save  separate 
samples  of  plain  and  molasses  pulp  if  both  are  produced  during  the 
same  week. 

PRKI-ARATION  OP  SAMPLE 

Mix  the  sample  well  with  the  hands  and  save  a  portion  for 
the  determination  of  moisture.  Crush  at  least  50  grams  of  the  re- 
mainder in  an  iron  *mortar,  crusher,  or  disc  pulverizer,  to  pass 
a  sieve  having  circular  openings  1  mm  in  diameter.  (Or  use  a 
regular  20-mesh  sieve.)  Preserve  both  samples  in  tight  containers. 

ANALYSIS 

Follow  the  methods  in  Chap.  XX,  ''Foods  and  Feeding 
Stuffs."  Determine  the  moisture  in  duplicate  in  both  the  original 
and  the  ground  material.  Make  all  other  determinations  on  the 
ground  material,  and  correct  the  results  for  the  loss  of  moisture 
during  grinding. 

For  example : 

Let  a  =  percentage  of  moisture  in  original  material 
b  =  percentage  of  moisture  in  ground  material 
c  =  percentage  of  crude  protein  in  ground  material 
x  =  percentage  of  crude  protein  in  original  material 

c  (100  — a) 

Then  x  = . L. 

100  — b 

NOTE 

As  the  amount  of  crude  fat  in  dried  pulp  is  small  and  very 
constant,  this  determination  may  be  omitted  on  the  weekly  samples, 
but  should  be  made  on  a  campaign  average  sample.  When  the 
crude  fat  is  not  determined,  allow  0.2  for  the  percentage  of  crude 
fat  in  calculating  the  nitrogen-free  extract. 

10.     TEMPERATURE  DATA 

GENERAL 

Refer  to  the  general  instructions  in  the  section  of  the  same 
title  in  Chapter  II,  36. 


*Flain  pulp  of  normal  moisture  content  can  be  easily  ground  in  a  disc 
pulverizer.     Molasses  pulp  is  best  crushed  in  an  iron  mortar. 


68  METHODS  OF  ANALYSIS 

MOLASSES  TO  PULP  DRYER 

Obtain  every  2  hours  from  the  line  leading  to  the  drying  drum. 

PULP  ENTERING  PRESSES 

Obtain  every  2  hours  the  temperature  of  the  pulp  just  previous 
to  entering  a  press  which  is  in  operation. 

GAS  LEAVING  FURNACE 

Obtain  from  the  recording  pyrometer  at  the  furnace. 

GAS  LEAVING  DRYER 

Obtain  from  the  recording  thermometer  at  the  exit  of  the  dryer. 


VI.     PULP  SILO  CONTROL 

1.     GENERAL 

Sample  and  analyze  "pulp  entering  silo"  once  a  day  during 
campaign.  Sample  and  analyze  "pulp  sold"  once  a  day  (except 
on  Sundays  and  holidays  during  intercampaign)  as  long  as  any 
unsold  pulp  is  on  hand,  but  only  on  days  when  wagons  are  being 
loaded  at  the  silo. 

2.     PULP  ENTERING  SILO 

Determine : 

(a)     Dry  Substance. 

SAMPLING 

Take  a  good-sized  sample  from  the  discharge  of  the  pulpe- 
fanger,  enough  to  fill  a  ten-quart  bucket  three-fourths  full,  in  such 
a  manner  as  to  obtain  as  nearly  as  representative  a  sample  as  pos- 
sible of  the  mixture  of  pulp  and  water  discharged  into  the  silo. 
Drain  in  a  "pulp  can"  as  in  the  case  of  "Pulp  Entering  Presses," 
Chapter  V,  5,  "Pulp  Dryer  Control." 

ANALYSIS 

Analyze  as  under  "Pulp  Entering  Presses,"  Chapter  V,  5, 
"Pulp  Dryer  Control." 

3.     PULP  SOLD 

Determine : 

(a)  Acidity. 

(b)  Dry  Substance. 

S  \MI-IJNG 

Take  three  samples  from  the  top  of  the  wall  of  pulp  where 
the  wagons  are  being  loaded ;  take  another  set  of  three  samples  from 


70  METHODS  OF  ANALYSIS 

the  middle;  and  take  a  third  set  of  three  samples  from  the  bottom. 
Mix  the  nine  samples  to  form  a  composite  sample  for  analysis. 

ANALYSIS 

(a)  Acidity:    Weigh  out  10  grams  of  the  well  mixed  sample, 
and  rinse  into  a  beaker  or  casserole  with  a  little  neutral,  distilled 
water.    Add  a  few  drops  of  phenolphthalein  and  then  N/28  alkali 
in  excess,  and  dilute  to  a  total  volume  of  about  200  ml.     Cover 
with  a  watch  glass  and  boil  gently  for  15  minutes.    Cool  and  titrate 
with  N/28  acid,  continuing  the  addition  of  the  acid  until  the  solu- 
tion remains  colorless  for  15  minutes.     The  amount  of  standard 
alkali  originally  added  should  be  such  that  not  less  than  5  ml  nor 
more  than  10  ml  of  the  standard  acid  is  subsequently  required  for 
neutralization.    Subtract  the  number  of  ml  of  acid  from  the  num- 
ber of  ml  of  alkali  used,  and  divide  by  100  to  obtain  the  acidity  (in 
terms  of  per  cent  CaO  by  weight). 

(b)  Dry  Substance:    Weigh  out  10  grams  of  the  sample,  the 
acidity  of  which  has  been  previously  determined  as  in  (a),  using  a 
tared  aluminum  moisture  dish  provided  with  a  cover  and  a  small 
glass  rod.    Add  8 — 10  ml  of  water  and  the  exact  weight  of  freshly 
ignited  C.  P.  calcium  oxide  indicated  by  the  acidity  test  to  be  re- 
quired for  neutralization.     Stir  with  heating  until  a  uniform  mix- 
ture is  obtained.     (Add  a  drop  of  phenolphthalein  to  show  when 
all  the  particles  of  pulp  have  come  in  contact  with  the  calcium 
oxide ;  the  phenolphthalein  will  retain  its  pink  color,  which  will  be 
uniformly  distributed   when   the  mixing  is   perfect).     Dry   in   a 
glycerin  oven  at  100 — 105°  for  5 — 6  hours,  and  then  for  successive 
periods  of  one  hour  until  the  loss  in  weight  in  any  period  is  less 
than  0.1%. 

Obtain   the   percentage    of   dry   substance   by   the    following 
formula : 

Let  a  =  weight  of  pulp  used 

b  =  acidity  of  pulp  (grams  of  CaO  in  100  ml) 

c  =  weight  of  dried  material 

x  ==  weight  of  CaO  required 

y  =  percentage  of  dry  substance 

Then  x  =  —^- 

100  (e  —  .68  x) 
Andy=- 


Or,  as  a  =  10, 

y  =  10  (c  —  .68  x) 


tt 

A  cl  I  HI 

the  use  of  Table  16. 


VI.      PULP  SILO  CONTROL  71 

y"  can  be  conveniently  obtained  by 


The  factor  .68  in  the  above  formulas  is  derived  as  follows:  Assuming 
acetic  acid  to  be  the  principal  acid  present,  the  acetic  acid  of  the  original 
material  is  converted  to  calcium  acetate  in  the  dried  sample  in  the  ratio 
of  the  molecular  equivalents,  i.  e.  of  120  to  158.  Then,  since  the  molecular 
equivalent  of  calcium  oxide  is  56,  (158  — 120)  -=-  56  =  .68,  which  repre- 
sents the  factor  by  which  the  amount  of  calcium  oxide  used  must  be  multi- 
plied to  obtain  the  deduction  necessary  to  convert  the  calcium  acetate 
back  to  free  acetic  acid. 


VII.     BOILER  HOUSE  CONTROL 

1.     GENERAL 

No  definite  routine  should  be  followed  in  the  boiler  house  con- 
trol work;  irregularity  in  the  time  of  sampling  and  testing  the  in- 
dividual boilers  will  tend  to  give  more  nearly  average  results.  The 
boiler  house  control  man  should  take  and  prepare  all  the  necessary 
coal  and  ash  samples,  make  the  flue  gas  analysis,  and  obtain  the 
draft  and  temperature  readings  and  any  other  necessary  data.  If 
a  boiler  house  control  man  is  not  employed,  the  man  in  charge  of 
unloading  the  coal  should  take  the  coal  samples,  and  the  Assistant 
Chemist  should  obtain  the  ash  samples;  the  other  data  on  flue  gas 
analysis  and  temperature,  draft,  etc.,  will  not  be  obtained  except 
for  what  average  figures  are  available  from  the  recording  instru- 
ments. 

2.     SAMPLING  OF  COAL 

Use  a  sampler  consisting  of  a  piece  of  2-inch  pipe  about  4  feet 
long,  provided  with  a  spring  valve  at  one  end  to  retain  the  coal 
in  the  sampler.  Sample  all  cars  unloaded,  just  previous  to  un- 
loading, by  driving  the  sampler  through  the  coal  in  the  car  and 
collecting  the  coal  retained  in  the  pipe.  Take  3  samples  from  each 
car,  one  in  a  corner  about  two  feet  equally  distant  from  the  sides 
of  the  car,  one  in  the  center  of  the  car,  and  one  in  the  corner 
diagonally  opposite  the  position  of  the  first  sample.  Preserve  all 
the  samples  in  a  can  provided  with  a  tightly  fitting  cover,  such  as 
a  milk  can,  or  in  a  number  of  such  containers,  and  keep  in  a 
cool  place. 

Sample  cars  loaded  from  the  storage  pit  in  the  same  manner 
as  cars  received  from  the  mine;  if  coal  is  hauled  from  the  storage 
piles,  take  one  sample  from  every  fifth  wagonload.  Take  no  samples 
from  cars  loaded  from  the  drippage  pit,  or  from  cars  into  which 
any  drippage  has  been  loaded;  pay  special  attention  to  this  point 


VII.       BOILER   HOUSE  CONTROL  73 

to  avoid  contaminating  the  regular  sample  with  drippage.  It'  coal 
Irom  different  sources  (mine,  storage  pit,  etc.)  is  being  used,  in- 
clude in  the  gross  sample  amounts  from  each  source  in  approximate 
proportion  to  the  amounts  from  each  source  used. 

Sample  the  coal  used  in  the  Pulp  Dryer  in  exactly  the  same 
manner.  The  sampling  should  be  done  in  this  case  by  the  man 
who  unloads  the  coal  for  the  dryer  but  should  be  under  the  super- 
vision of  the  boiler  house  control  man. 

3.  PREPARATION  OF  COAL  SAMPLES 

When  all  the  coal  for  a  day's  use  has  been  sampled,  crush  the 
entire  gross  sample  to  Vi-inch  size  and  reduce  to  1  to  2  quarts  by 
mixing  and  quartering  on  a  large  piece  of  canvas;  do  this  as  rap- 
idly as  possible  to  avoid  loss  of  moisture.  Keep  the  sample  in  a 
fruit  jar  closed  with  a  tightly  fitting  cover  provided  with  a  rubber 
gasket. 

At  the  end  of  the  week  grind  the  entire  seven  samples  repre- 
senting the  week's  run  of  coal  to  60-mesh  size  in  the  pebble  mill 
described  in  Chap.  XXIII,  9.  Put  up  and  seal  a  4-oz.  sample  of 
the  ground  material,  and  forward  it  without  delay  to  the  central 
laboratory  for  analysis.  Be  careful  to  clean  the  mill  thoroughly 
after  each  week's  sample  is  prepared,  and  employ  it  exclusively  for 
grinding  coal. 

4.     SAMPLING  OF  ASHES 

(a)     IN  BOILER  HOUSES  EQUIPPED  WITH  CHAIN  GRATE  STOKKUS 
Obtain  samples  of  grate1  and  flume  ashes  as  follows : 

(1)  Grate  (Stoker)  Ash :     I'M-  a  sampler  consisting  of  a  rec- 
tangular box  with  hinged  cover  fastened  to  a  long  handle.     Obtain 
3  samples  per  shift,  if  possible,  from  the  discharge  of  each  stoker 
in  operation,  taking  a  sufficient  quantity  so  that  the  total  sample 
for  the  8  hours  will  amount  to  about  one  gallon.     Save  separate 
samples  for  each  shift  for  the  set  of  boilers  in  charge  of  each  fire- 
man.    This  will  make  6  samples  per  24  hours  at  the  large  factories 
and  3  at  the  small  factories. 

(2)  Flume  Ash:     Obtain   the  sample  by  holding  a  closely 
woven  sack  over  the  discharge  of  the  flume  ash  line,  or  over  the 
special  sampler  provided  for  this  purpose,  in  such  a  manner  as  to 
obtain  an  average  of  all  solid  material  delivered  through  the  line. 
Take  a  sample  at  least  twice  a  shift  and  make  up  a  composite 


74  METHODS  OF  ANALYSIS 

sample  for  each  shift  by  mixing  at  least  1  quart  of  each  of  the  in- 
dividual samples. 

(b)  IN  BOILER  HOUSES  EQUIPPED  WITH  HAND  FIRED  FURNACES 
Obtain  samples  of  pan,  grate,  and  flume  ashes  as  follows : 

(1)  Pan  Ash:    Take  a  small  sample  of  the  ash  in  the  pan  of 
each  boiler  in  operation  at  least  3  times  per  shift ;  the  total  sample 
for  the  shift  should  be  about  one  gallon.     Save  separate  samples 
for  each  shift.    If  a  boiler  house  control  man  is  not  employed,  ob- 
tain a  1-quart  sample  once  a  shift  representing  an  average  of  the 
ash  in  the  pans  at  the  time  of  sampling. 

(2)  Grate  Ash:    Take  samples  only  when  the  fires  are  being 
pulled  and  before  the  ash  is  wet  down.     Obtain  an  average  sample 
of  at  least  1  gallon  once  a  shift,  or  oftener  if  a  boiler  house  control 
man  is  employed.    Crush  the  gross  sample  to  break  up  large  lumps, 
mix,  and  save  a  1-quart  sample  representing  the  work  of  each  shift. 

(3)  Flume  Ash:    Obtain  at  least  twice  a  shift  as  described  in 
11  (a),  (2),"  above.    If  a  boiler  house  control  man  is  not  employed, 
obtain  at  least  once  a  shift. 

(c)  IN  PULP  DRYERS 

The  boiler  house  control  man  or  the  Assistant  Chemist  should 
obtain  an  average  sample  of  the  grate  ash  at  least  once  per  shift, 
as  described  in  (a)  (1). 

5.     PREPARATION  OF  ASH  SAMPLES 

Break  up  any  large  lumps  by  crushing,  mix  well,  take  out 
1  quart  and  crush  to  10  mesh  size  in  a  jaw  crusher.  Mix  the 
crushed  sample  and  grind  at  least  one-fourth  of  it  to  60  mesh 
size  in  a  disc  pulverizer.  Mix  well  and  save  4  ounces  for  analysis. 

As  the  samples  of  ash  are  analyzed  on  a  dry  basis,  no  care 
need  be  taken  to  avoid  loss  or  gain  of  moisture  during  the  prepara- 
tion of  the  sample.  Any  samples  which  are  very  wet,  however, 
such  as  the  flume  ashes,  should  first  be  dried  in  a  shallow  tray  in 
a  warm  place  before  being  prepared  for  analysis. 

If  the  special  boiler  house  control  is  carried  on,  the  samples 
of  ashes  collected  to  represent  the  work  of  each  shift  should  be 
analyzed  separately.  Otherwise  a  composite  sample  of  each  kind 
of  ashes  should  be  prepared  at  the  end  of  every  week  and  sent  to 
the  central  laboratory,  together  with  the  coal  sample,  for  analysis. 
See  Chapter  XV,  10,  regarding  the  analysis  of  ash  samples. 


VII.      BOILER  HOUSE  CONTROL  75 

6.     DRAFT 

Take  draft  readings,  both  "furnace"  and  "differential,"  on 
the  individual  boilers  at  the  time  when  samples  of  the  grate  ash 
are  collected.  Check  all  the  draft  gages  at  the  zero  point  at  least 
once  a  shift,  and  test  all  connections  for  air  leaks  frequently. 

The  liquid  used  in  Ellison  and  in  Blouck  differential  draft 
gages  is,  unless  otherwise  specified,  mineral  oil  of  .834  specific 
.irravity  at  60°  F.,  colored  red  or  blue.  The  best  temporary  substi- 
tute is  kerosene,  having  nearly  the  same  specific  gravity.  Water 
must  not  be  used. 

In  the  absence  of  a  boiler  house  control  man  or  the  necessary 
differential  gages,  no  readings  will  be  recorded. 

7.     FLUE  GAS  ANALYSIS. 

Immediately  after  the  ash  sample  is  taken  and  the  draft  read- 
ings are  made,  determine  the  percentage  of  carbon  dioxide  in  the 
flue  gas,  using  an  Orsat  apparatus  or  one  of  the  modified  forms 
of  the  same,  and  following  the  method  prescribed  for  the  analysis 
of  lime  kiln  gas,  Chap.  II,  10.  Change  the  caustic  alkali  solution 
every  2  days.  The  addition  of  a  few  drops  of  phenolphthalein  to 
the  water  in  the  measuring  burette  will  be  of  value  to  indicate 
contamination  from  the  alkali  solution.  Rinse  out  the  sampling 
pipe  thoroughly  before  drawing  gas  into  the  apparatus.  Do  not 
make  any  flue  gas  analyses  on  banked  boilers. 

The  gas  sampling  pipe  should  pass  through  a  hole  drilled  in 
the  brickwork,  and  the  open  end  through  which  the  gas  enters 
should  be  close  to  the  point  where  the  gases  leave  the  boiler  and 
where  the  velocity  of  the  gas  stream  is  a  maximum.  Leakage 
around  the  sampler  should  be  stopped  with  asbestos  packing.  The 
proper  position  of  the  sampler  is  of  great  importance. 

It  is  also  advisable,  especially  when  the  C02  is  high,  to  make 
some  complete  analyses  in  which  oxygen  and  carbon  monoxide 
(CO)  are  determined. 

In  the  absence  of  the  special  boiler  house  control,  no  indi- 
vidual flue  gas  analyses  will  ordinarily  be  made. 

8.     TEMPERATURE  OF  AIR  AND  FLUE  GAS 

(a)     AIR  ENTERING  FURNACES 

Take  readings  at  the  time  when  the  flue  gas  is  analyzed,  of 
thermometers  in  different  parts  of  the  boiler  room  hung  near  the 


76  METHODS  OF  ANALYSIS 

point  where  the  air  enters  below  the  stokers  but  not  so  close  that 
they  will  be  heated  by  radiation  from  the  fire. 

(b)     FLUE  GAS 

If  the  boilers  are  equipped  with  individual  thermometers  01? 
if  a  suitable  pyrometer  is  available,  determine  the  temperature  of 
the  flue  gas  at  the  point  where  it  leaves  the  boiler  at  the  time  when 
the  gas  is  analyzed.  If  only  a  general  recording  instrument  is 
available,  take  several  readings  during  the  period  of  ash  sampling 
and  gas  analysis,  and  use  the  average  of  these  readings  as  a  basis 
for  figuring  the  heat  loss. 

9.'    CALCULATION  OF  HEAT  LOSSES 

(a)  DATA  REQUIRED 

(1)  Moisture,  Ash,  and  Calorific  Value  of  Coal.    On  account 
of  the  fact  that  the  results  of  the  coal  analysis  are  not  available 
until  several  days  after  the  samples  are  taken  and  then  only  for 
weekly  samples,  use  the  average  analysis  to  date  of  the  coal  burned 
during  the  campaign,  recalculating  these  averages  when  each  new 
set  of  figures  is  received  from  the  central  laboratory.     During  the 
first  few  days  of  the  campaign,  or  until  figures  have  been  received 
from  the  central  laboratory,  use  the  average  coal  analysis  of  the 
preceding  campaign. 

(2)  Carbon   and  Hydrogen   in    Coal.     Use   average   figures 
obtained  from  the  analyses  of  the  Bureau  of  Mines.     (See  refer- 
ences in   Section  10.)      For  northern   Colorado  lignite    (sub-bitu: 
minous)    coal  the  percentage  of  carbon  may  be  taken  as  57  and 
the  percentage  of  hydrogen  as  6,  if  the  amount  of  combustible  is 
approximately  75  per  cent. 

(3)  Other  data  required  are  obtained  from  the  daily  deter- 
minations. 

(b)  Loss  IN  DRY  FLUE  GAS 

Obtain  from  the  chart  (^drawing  S-1756  or  S-132-M)  the 
"B.  T.  U.  lost  in  dry  flue  gas  per  pound  of  carbon  burned," 
according  to  the  average  flue  gas  analysis,  and  the  average  tern- 
perature  of  the  air  and  of  the  flue  gas. 


*The  Lovell  factory,  where  natural  gas  is  used,  should  employ  the 
chart  in  drawing  S-126-M. 


VII.      BOILER  HOUSE  CONTROL  77 

Let  T  =  temperature  (°  F)  of  flue  gas 

t  =  temperature  (°  F)  of  air  entering  furnaces 
B  =  B.  T.  U.  found  from  the  chart 
A  =  calorific  value  (B.  T.  U.)  of  the  coal  as  fired 
C  =  %  carbon  in  coal  as  fired 
L1  =  percentage  loss  of  heat  in  dry  flue  gas 

Then  Ll  =  _°B 
A 

EXAMPLE 

Assume  12%  C02  in  flue  gas  and  temperature  of  500°  F., 
boiler  room  temperature  of  80°  F.,  and  9000  B.  T.  U.  in  coal  con- 
taining 57%  carbon.  From  the  chart  T  —  t  =  420,  and  B  =  2120. 

57  X  2120 

L,  =  =  ±0.4 

9000 

For  coal  containing  57%  carbon,  the  calculation  may  be  short- 
ened by  the  use  of  Table  17.  The  value  found  in  the  table  multi- 
plied by  100  and  divided  by  the  B.  T.  U.  in  the  coal  gives  the 
percentage  loss  desired.  If  the  percentage  of  carbon  in  the  coal 
is  not  taken  as  57,  the  table  may  still  be  used  by  multiplying  by 

C1 
a  factor  equal  to  —  ,where  C  is  the  percentage  of  carbon  in  the 

57 
coal. 

EXAMPLE 
For  12%  COo  and  T  —  t  =  420,  Table  17  gives  1208  B.  T.  U. 

Then    1208X1Q°     =13.4 

9000 

Note  that  the  chart  gives  "B.  T.  U.  per  pound  of  carbon 
burned"  and  the  table  "B.  T.  U.  per  pound  of  coal  burned." 

(c)     Loss  DUE  TO  MOISTURE 

The  loss  due  to  moisture  is  composed  of: 

(1)  Loss  due  to  moisture  in  the  coal  as  fired. 

(2)  Loss  due  to  moisture  resulting  from  the  *burning  of  the 
hydrogen  component  of  the  fuel. 

In  addition  to  the  symbols  previously  used, 
Lot  M  =  %  moisture  in  coal  as  fired 
H  =  %  hydrogen  in  coal  as  fired 


*The  Lovell  factory,  where  natural  gas  is  used,  should  calculate  this 
loss  in  accordance  with  the  chart  in  drawing  S-153-M. 


78  METHODS   OF  ANALYSIS 

w  =  boiling  point   (°  F.)   of  water  (202  for  5000  feet 

elevation) 
L2  =  percentage  loss  of  heat  due  to  moisture 

Then  L2  =   M  +  9  H    x  [(w  —  t)  +  976.6  +  .47  (T  —  w)] 
A 

EXAMPLE 

Assume  in  addition  to  the  figures  in  the  preceding  example, 
16%  moisture  and  6%  hydrogen  in  the  coal,  and  boiling  point  of 
water  as  202°  F. 

(16  +  54)  X  [122  +  976.6  +  .47  (500  —  202)] 

jj    =   -  _____  -  _  __  y^ 

9000 

This  calculation  may  be  shortened  as  follows  by  the  use  of 
Tables  18  and  18—  A. 

Let  F  =  factor  as  found  in  Table  18. 
F'  =  factor  as  found  in  Table  18  —  A. 

FF' 
Then  L2  = 

A 

EXAMPLE 

According  to  the  data  previously  given,  F  =  70.0  and 
F'  =  1239 


Then  L,=  =  9.6 

9000 

(d)  TOTAL  Loss  IN  FLUE  GAS 

Let  L3  =  total  percentage  loss  of  heat  in  flue  gas 
Then  L3  =  L,  +  L2 

EXAMPLE 
L3  =  13.4  +  9.6  =  23.0 

(e)  Loss  DUE  TO  COMBUSTIBLE  IN  ASH 

This  is  based  on  the  analysis  of  the  coal  and  of  the  grate 
(stoker)  ashes,  the  combustible  matter  in  the  ashes  being  assumed 
to  consist  of  pure  carbon  of  a  calorific  value  of  14600  B.  T.  IT. 

Let  D  =  %  ash  in  coal  as  fired 
E  =  %  ash  in  ashes 

L4  =  percentage  loss  of  heat  due  to  combustible  in  ashes 
14600  D   (100  —  E) 


Then  L4  = 


A  E 


VII.      BOILER  HOUSE  CONTROL  79 


14600  D 
Or  it  k  =F  -  _  -  a  factor  which  can  be  used  for  a  number 

A 

of  calculations 


E 

EXAMPLE 

Assume  the  coal  to  contain  12%  ash,  and  the  ashes  60%  ash. 
14600X12X40    =13Q 

9000  X  60 
(f)     TOTAL  KNOWN  LOSSES 

If  L5  =  total  known  heat  losses, 
Then  L5=L3  +  L4 

EXAMPLE 
L5  =  23.0  +  13.0  =  36.0 

10.     BIBLIOGRAPHY 

11  Sampling1  and  Analyzing  Flue  Gas"  —  Bur.  Mines,  Bulletin  97. 
"Combustion  and  Flue  Gas  Analysis"  —  Bur.  Mines,  Tech.  Paper 

219. 
"Apparatus  for  the  Exact  Analysis  of  Flue  Gas"  —  Bur.  Mines, 

Tech.  Paper  31. 
"Measuring  the  Temperature  of  Gases  in  Boiler  Settings"  —  Bur. 

Mines,  Bulletin  145. 
U.  S.  Geological  Survey  Professional  Paper  48,  and  Bur.  Mines 

Bulletins  22,  85,  and  123  —  Analyses  of  mine  and  car  samples 

of  coals  of  the  United  States,  1904  —  1916. 
"Steam"—  Babcock  &  Wilcox  Co.,  New  York. 


VIII,    POTASH  CONTROL  (BEET  CAMPAIGN) 

1.     GENERAL 

Each  factory  engaged  in  potash  recovery  should  send  to  the 
Central  Laboratory  weekly  average  samples  of  Molasses  Worked, 
Saccharate  Cake,  and  Total  Waste  Water,  which  should  represent, 
in  each  case  an  average  of  all  laboratory  samples  taken  during  the 
week,  as  described  in  Chapter  II,  35,  "Weekly  Composite  Sam- 
ples. "  The  samples  and  information,  as  specified  in  detail  below, 
should  be  forwarded  to  the  Central  Laboratory  as  soon  as  possible 
after  the  end  of  every  week,  at  least  not  later  than  Monday  noon. 

(a)  MOLASSES  WORKED 

Forward  100  grams  of  the  average  sample  of  the  molasses 
worked  during  the  week. 

(b)  SACCHARATE  CAKE 

Forward  an  amount  equivalent  to  100  grams  of  dry  substance, 
of  an  average  sample  of  Saccharate  Cake,  representing  a  weighted 
average  of  the  cold  and  hot  cakes  made  up  as  in  the  following 
example : 

Brix  of  Cold  Saccharate  Cake 62.0 

Brix  of  Hot  Saccharate  Cake 55.0 

Tons  of  Dry  Sub.  in  Cold  Saccharate  cake  for  Week 450 

Tons  of  Dry  Sub.  in  Hot  Saccharate  Cake  for  Week 60 

Tons  of  Dry  Sub.  in  Total  Saccharate  Cake  for  Week 510 

Then  the  number  of  grams  of  the  original  material  of  Cold 
Cake  to  be  used  for  the  sample  is 

450  100    _H23 

510  .620 

And  the  number  of  grams  of  IJot  Cake  is 


510  .550 


VIII.       POTASH    CONTROL    (BEET   CAMPAIGN)  81 

The  material  referred  to  above  is  of  course  the  syrup  obtained 
after  the  carbonation  and  evaporation  of  the  cake  from  the  saccha- 
rate  presses. 

(c)  TOTAL  WASTE  WATER 

Forward  100  grains  of  the  weekly  average  samples. 

(d)  DATA  REQUIRED 

Forward  also  the  following  data,  both  for  the  week  and  to 
date: 

Tons  of  Molasses  Worked. 

%  Sugar  in  Molasses  Worked. 

Sugar  in  Total  Waste  Water,  per  cent  on  Sugar  in  Molasses 
Worked. 

Cubic  Feet  of  Total  Waste  Water  Produced. 

Cubic  Feet  of  Waste  Water  Actually  in  Reservoir. 

Total  Waste  Water,  Brix. 

Total  Waste  Water,  Alkalinity. 

Total  Waste  Water,  Sugar. 

2.    ANALYSIS 

The  Central  Laboratory  will  make  the  necessary  analyses  ac- 
cording to  the  standard  methods  described  in  Chapter  IX,  12,  and 
elsewhere  in  the  "Methods  of  Analysis/' 


IX.  POTASH  CONTROL  (POTASH  CAMPAIGN) 

This  chapter  relates  to  the  laboratory  control  work  which  is 
to  be  carried  on  during-  the  potash  campaign  at  every  factory 
engaged  in  potash  recovery. 

1.     LIQUOR  ENTERING  FACTORY 

Determine  every  4  hours : 

(a)  Brix. 

(b)  Alkalinity. 

(c)  Sugar. 

SAMPLING 

Take  a  catch  sample  every  4  hours  from  the  line  from  the 
reservoir  to  the  factory  before  the  liquor  has  passed  through  any 
heater. 

ANALYSIS 

Determine  as  in  the  case  of  Steffen  Waste  Water,  Chap.  IV,  6. 

2.     FIRST  SATURATION  LIQUOR 

Determine  every  hour  : 
(a)     Alkalinity. 

• 

SAMPLING 

Take)  a  cateh  sample  from  the  cocks  or  troughs  of  the  first 
presses,  avoiding  any  admixture  of  wash  water. 

ANALYSIS 

Determine  the  alkalinity  in  the  regular  manner  with  N/28 
acid. 

NOTE  :  If  double  carbonation  is  not  employed,  this  determina- 
tion is  necessarily  omitted. 


IX.       POTASH  CONTROL   ( POTASH  CAMPAIGN)  83 

3.     THIN  LIQUOR  ENTERING  EVAPORATORS 

Determine  every  4  hours: 

(a)  Brix. 
Determine  every  hour: 

(b)  Alkalinity. 

(c)  Reaction  with  CO2. 

SAMPLING 

Take  a  catch  sample  from  the  pump,  or  at  a  suitable  point  in 
the  line  between  the  filters  and  the  evaporators. 

ANALYSIS 

(a)  Brix:    Determine  in  the  regular  manner. 

(b)  Alkalinity:    Determine  as  in  the  case  of;  " First  Satura- 
tion Liquor." 

(c)  Reaction  with  C02:    Pass  carbon  dioxide  gas  for  a  few 
minutes  through  a  portion  of  the  sample  in  a  1  x  6  inch  test  tube. 
If  any  cloudiness  results,  report  as  "P"  indicating  the  formation 
of  a  precipitate,  and  if  no  cloudiness  appears  report  as  "0." 

4.     EVAPORATOR  THICK  LIQUOR  PRODUCED 

Determine  every  4  hours: 

(a)  Brix. 
Determine  every  24  hours : 

(b)  Sugar. 

SAMPLING 

Take  a  sample  from  the  pump,  or  from  the  line  to  the  potash 
scale  tank.  Do  not  take  the  sample  from  the  last  body  of  the 
evaporators  or  from  the  scale  tank.  Take  a  sample  each  time  when 
liquor  is  let  out  of  the  evaporators,  and  composite  equal  portions 
of  the  individual  samples. 

ANALYSIS 

(a)  Brix:    Follow  the  "General  Methods,"  1  (a). 

(b)  Sugar:    Transfer  13  grams  to  a  100  ml  flask,  add  a  few 
drops  of  phenolphthalein,  and  neutralize  with  dilute  acetic  acid. 


84  METHODS  OF  ANALYSIS 

Add  4 — 6  ml  of  basic  lead  acetate,  make  up  to  the  mark,  filter,  and 
polarize  in  a  200  mm  tube.    Multiply  the  reading  by  2. 

5.  FILTER  PRESS  CAKE 

Determine  every  8  hours : 
(a)     Weight  per  cake. 

SAMPLING 

Take  a  representative  sample  at  least  every  8  hours  in  the 
manner  described  in  Chap.  II,  13,  "Lime  Cake."  Save  equal  por- 
tions for  the  weekly  composite  sample  described  below. 

DETERMINATION 

Determine  the  average  weight  of  one  cake  in  pounds  once  a 
shift  by  catching  and  weighing  two  or  three  cakes  taken  at  random. 
In  the  case  of  Kelly  presses  the  amount  of  cake  is  best  calculated 
from  the  difference  in  alkalinity  between  the  original  and  car- 
bonated liquor  and  the  CaO  content  of  the  cake. 

6.  CONDENSED  WATERS 

Examine,  by  the  *alpha-naphthol  test,  the  boiler  feed  water 
every  hour,  and  the  press  wash  and  evaporator  tail  pipe  waters 
every  2  hours.  Test  also  the  drips  from  each  evaporator  body  as 
frequently  as  practicable. 

See  Chap.  XVII,  2  (c)  regarding  the  collection  of  campaign 
samples  for  analysis. 

7.     BOILER  WATER 

Determine  every  8  hours  on  each  boiler  in  service : 
(a)     Alkalinity. 

SAMPLING 

Draw  from  the  sampling  line,  first  allowing  the  water  to  run 
a  few  moments  to  rinse  out  the  pipe. 

ANALYSIS 

Measure  out  10  ml  with  a  pipette  into  a  porcelain  dish  and 
follow  the  "General  Methods,"  I,  10  (a),  using  phenolphthalein 


'See  Chapter  I,  13. 


IX.   POTASH  CONTROL  ( POTASH  CAMPAIGN)  85 

as  indicator.    Dilute  with  sufficient  neutral  water  to  make  the  coloi 
reaction  distinct. 

8.     CAEBONATION  GAS 

Determine  every  4  hours: 
(a)     C02. 

SAMPLING  AND  ANALYSIS 

Obtain  the  sample  and  determine  the  percentage  of  C02  as 
described  in*  Chap.  II,  10,  "Lime  Kiln  Gas. 


?  ? 


9.     EVAPORATOR  THICK  LIQUOR  ENTERING  FURNACE 

Determine  every  2  hours: 

(a)  Brix. 

I  )rt  ermine  every  24  hour- : 

(b)  Dry  Substance. 

(c)  Lixiviated  Ash. 

SAMPLING 

Take  a  sample  every  2  hours  from  the  line  leading  from  the 
storage  tank  to  the  furnace.  Make  up  a  composite  sample  for  the 
dry  substance  and  ash  determinations. 

ANALYSIS 

Follow  the  "General  Methods." 

10.     CRUDE  ASH  AS  SACKED 

Determine  every  24  hours: 

(a)  Acid  Insoluble. 

(b)  Lixiviated  Ash. 

SAM  i 'LING 

The  man  at  the  sacking  station  should  take  a  small  measureful 
from  each  bag  filled  and  transfer  it  to  a  covered  container.  A 
laboratory  employe  should  mix  the  gross  sample  well  and  transfer 
a  suitable  amount  to  a  tightly  stoppered  bottle. 

If  the  material  is  shipped  as  fast  as  it  is  sacked,  this  sampling 
'•an  be  combined  with  the  collection  of  samples  representing  each 
ear-load  lot  described  in  Chapter  X. 


86  METHODS  OF  ANALYSIS 

ANALYSIS 

(a)  Acid  Insoluble  and  (b)  Lixiviated  Ash:  Follow  the 
methods  given  under  "Crude  Potash,"  Chap.  X,  6  and  8. 

11.     TEMPERATURE  DATA 

Take  readings  every  2  hours  of  the  thermometers  indicating 
the  temperature  of  the  liquor  entering  and  leaving  each  set  of 
heaters;  record  also  the  kind  of  steam  or  vapor  used  in  each  case. 
Take  readings  also  every  2  hours  of  the  temperature  of  the  liquor 
in  each  body  of  the  evaporators. 

12.     WEEKLY  COMPOSITE  SAMPLES 

SAMPLING 

Make  up  a  composite  sample  of  each  of  the  products  mentioned 
below  by  taking  equal  portions  of  each  sample  brought  to  the  lab- 
oratory during  the  week  and  preserving  in  a  sealed  jar  or  stoppered 
bottle. 

(a)  LIQUOR  ENTERING  FACTORY 

Determine  dry  substance  (after  carbonation)  and  K20. 

(b)  THIN  LIQUOR  ENTERING  EVAPORATORS 
Determine  dry  substance  and  K20. 

(c)  FILTER  PRESS  CAKE 
Determine  dry  substance  and  K20. 

(d)  EVAPORATOR  THICK  LIQUOR  PRODUCED 

Determine  dry  substance,  lixiviated  ash,  K20,  and  NH3. 

(e)  CRUDE  ASH  AS  SACKED 

Determine  lixiviated  ash,  K20,  and  NH3. 

ANALYSIS 

(1)  Dry  Substance:  Determine  in  uncarbonated  liquors 
(waste  water  entering  factory)  as  follows:  Transfer  50  ml  to  a 
100  ml  flask  and  carbonate  at  80°  to  faint  alkalinity  with  phenolph- 
thalein.  Heat  .to  at  least  85°,  cool,  and  make  up  to  the  100  ml 
mark.  Mix  and  filter  through  a  dry  filter.  Determine  the  dry 
substance  in  the  filtrate  by  drying  on  sand  according  to  the  ' '  Gen- 
eral Methods, ' '  Chap.  I,  2.  Double  the  percentage  found  to  obtain 
the  percentage  in  the  original  liquor. 


IX.   POTASH  CONTROL  (  POTASH  CAMPAIGN)  87 

Determine  in  "thin  liquor  entering  evaporators"  and  in  thick 
liquor  by  drying  on  sand  without  preliminary  carbonation. 

Determine  in  filter  press  cake  by  drying  10  grams  directly  as 
in  the  case  of  Saccharate  Cake,  Chap.  IV,  11  (g). 

(2)  Lixiviated  Ash:     Follow    the    "General   Methods,"    I, 
7  (b). 

(3)  Potash   (K20):       Directions  for  the  determination  in 
crude  ash  will  be  found  in  Chap.  X,  9. 

In  the  case  of  liquors  and  filter  press  cake  proceed  as  follows: 
\\Vifrh  out  a  suitable  amount  (20  grams  of  thin  liquors,  1  gram 
of  thick  liquor,  and  10  grams  of  filter  press  cake)  in  a  platinum 
dish,  add  a  little  water  and  1  ml  of  sulphuric  acid  (1  to  1).  Evapo- 
rate on  a  water  bath  and  heat  cautiously  on  a  *Hillebrand  radiator 
until  the  sulphuric  acid  is  expelled.  Then  ignite  at  a  dull  red  heat 
until  the  ash  is  white.  Add  a  little  strong  hydrochloric  acid,  warm 
slightly  in  order  to  loosen  the  mass  from  the  dish,  and  dissolve 
in  about  25  ml  of  water.  Add  a  slight  excess  of  ammonium 
hydroxide,  heat  to  boiling,  and  add  sufficient  ammonium  oxalate 
to  precipitate  all  the  lime  present.  After  standing  for  at  least 
one-half  hour,  filter,  and  wash  well  with  hot  water.  Then  proceed 
as  in  the  determination  of  potash  in  crude  ash,  Chap.  X,  9. 

(4)  Nitrogen   as   Ammonia    (NHZ):     Determine    the    total 
nitrogen  as  in  the  analysis  of  crude  potash,  Chap.  X,  10. 

13.     STEAM  CALCULATION 

Calculate  a  heat  balance  every  week.  The  manner  of  calcu- 
lating- the  heat  units  in  the  steam  theoretically  required  can  best  be 
explained  by  the  following  example,  which  is  based  on  100  kilo- 
grams of  waste  water  entering  the  factory.  The  value  of  the 
latmt  heat  of  steam  is  taken  as  540  calories  per  kilogram  or  971 
B.  T.  U.  per  pound. 

Live  or         1st  2nd 

Exhaust     Vapor      Vapor 

HKATKRS  BEFORE  CARBONATIOX 


to 


100  kg  of  liquor  heated   from    10 

(80-10) 


*See  Chap.  XXIII,  15. 


88  METHODS  OF  ANALYSIS 

HEATERS  AFTER  CARBONATION  OR  AT  CARBONATION 

Live  or         1st  2nd 

Exhaust      Vapor      Vapor 
100  kg  of  liquor   heated   from   75° 
to  90°  10°   (90  —  75)  _ 
540 

HEATERS  BETWEEN  PRESSES  AND  EVAPORATORS 

Quantity  =  Weight  of  liquor  plus 
weight  of  wash  water  minus  (lime 
cake  minus  C02)  ==103'  kg.  103  kg 
of  liquor  heated  from  85°  to  105° 

103  (105  —  85) 

: _  =  3.8  kg  1st  vapor.  3.8 

540 

HEATING  IN  EVAPORATORS 

103  kg  of  liquor  heated  in  1st  body 
from  105°  to  110° 

103   (110  —  105) 

1 L  =  1.0   kg   exhaust    1.0 

540  

Totals    1.0  6.6  13.0 

EVAPORATION 

Assume  that,  according  to  actual  scale  weights,  6.0  kg  of  thick 

liquor  has  been  produced  per  100  kg  of  thin  liquor  introduced. 
Then  kg  of  water  evaporated  =  103  —  6.0  =  97.0 
Another  method  by  which  the  amount  of  evaporation  may  be 

calculated  is  from  the  percentage  of  dry  substance  in  the  thin  and 

thick  liquors. 

STEAM  CONSUMPTION  kg  of 

Steam 

97.0  total  kg  of  water  evaporated 
6.6  kg  evaporated  single  effect 6.6 

90.4 

26.0  kg  evaporated  double  effect  (2  X  13.0) 13.0 

64.4  kg  evaporated  quintuple  effect 12.9 

32.5 
Live  or  exhaust  steam  used  for  heating 1.0 

Total  Steam  Required 33.5 


IX.   POTASH  CONTROL  ( POTASH  CAMPAIGN)  89 

The  total  strain  theoretically  required  is  then  33.5  kg  per  100 
kg  of  thin  liquor,  or  33.5  tons  per  100  tons  of  thin  liquor  intro- 
duced. 

Now  let  A  =  tons  of  thin  liquor  introduced. 

B  =  tons  of  steam   required   per    100   tons   of   thin 

liquor  (33.5  in  the  above  example). 
C  =  tons  of  coal  burned. 

D  =  calorific  value  (B.  T.  U.  per  Ib.)  of  coal  burned. 
X  =  B.  T.  U.  theoretically  required. 
Y  =  B.  T.  U.  in  coal  burned. 

Then  tons  of  steam  required  is  - 

100 

And       X  =  _^? .  X  2000  X  971  =  19420  AB 
100 

where  971  is  the  latent  heat  of  steam  in  B.  T.  U.  per  pound, 
Also         Y  =  2000  CD. 

The  ratio  of  X  to  Y  is  then  a  measure  of  the  combined  effi- 
ciency of  the  boiler  house  and  the  heat  utilization. 


X.     CRUDE  POTASH 

1.     SAMPLING 

Take  a  large  sample  representing  each  car  of  crude  ash 
shipped.  If  the  potash  is  shipped  at  the  time  when  it  is  sacked, 
obtain  the  sample  by  taking  a  small  measureful  from  each  sack 
before  it  is  sewed,  until  the  number  of  sacks  required  to  load  the 
car  has  been  filled.  A  suitable  measure  can  be  made  by  riveting 
a  handle  on  a  20  ml  sheet  iron  crucible,  or  a  tin  measure  of  similar 
size  (38  x  32  mm)  may  be  used. 

If  the  potash  is  not  shipped  at  the  time  when  it  is  sacked, 
obtain  the  sample  at  the  time  of  shipment  by  drawing  a  sample 
from  each  bag  by  means  of  a  suitable  trier,  preferably  of  the  "In- 
diana type."  The  latter  consists  of  two  telescoping,  slotted  brass 
tubes  terminating  in  a  solid,  pointed  end.  This  enables  the  sampler 
to  be  inserted  full  length  into  the  bag  before  any  material  can 
enter  the  sample  chamber.  The  latter  is  then  opened  and  the 
sample  is  allowed  to  flow  in,  whereupon  the  sampler  is  closed  and 
then  withdrawn,  so  that,  a  complete  core  of  the  entire  bag  is  re- 
moved. The  sampler  should  be  about  18  inches  long,  or  long 
enough  to  extend  all  the  way  through  the  bag. 

Transfer  the  samples,  as  they  are  taken,  in  every  case  to  a 
covered  container,  and  employ  every  possible  precaution  to  pre- 
vent unnecessary  exposure  to  the  air. 

2.     PREPARATION  OF   SAMPLES 

(a)     GENERAL  METHOD 

Reduce  the  gross  sample  to  two  portions  of  about  2  pounds 
each  by  means  of  a  riffle  sampler.  Save  one  of  these  portions 
for  the  screen  test.  Reduce  the  other  portion  further,  and  put 
up  three  4  ounce  samples  and  seal  them  immediately,  as  described 


X.      CRUDE  POTASH  91 

below.  Handle  the  sample  as  rapidly  as  possible  throughout  in 
order  to  prevent  absorption  of  moisture.  See  section  3*  regarding 
the  further  preparation  of  the  sample  for  analysis. 

(b)  OPTIONAL,  METHOD 

This  method  may  be  used  only  for  crude  ash  consigned  within 
the  company  for  refining  or  other  purposes,  and  not  for  fertilizer 
material  sold  to  other  concerns. 

Proceed  as  in  (a)  up  to  the  point  where  the  sample  is  reduced 
to  two  portions  of  about  2  pounds  each.  Save  one  of  these  for 
the  screen  test,  as  before,  but  grind  the  other  portion,  the  full  2 
pounds,  in  a  porcelain  *pebble  mill  for  two  hours,  or  sufficiently 
long  to  reduce  it  to  60  mesh  size.  After  grinding,  open  the  mill 
and  put  up  immediately  the  three  samples  described  below. 

(c)  DESCRIPTION  OP  SAMPLES 

Put  up  three  samples  for  each  car,  labeled  with  the  name  of 
the  factory,  the  name  and  address  of  the  consignee,  the  car  number, 
the  weight  of  material,  and  the  date  of  shipment.  Designate  them 
respectively  "Seller's  No.  1,"  "Seller's  No.  2,"  and  "Seller's  No. 
3."  Save  an  additional  sample  of  the  unground  material  for  the 
screen  test,  as  previously  described. 

Use  "Seller's  No.  1"  sample  for  the  local  laboratory  analysis, 
and  seal  and  save  for  future  reference  the  portion  of  this  sample 
left  over  from  the  analysis.  Hold  the  other  two  seller's  samples 
subject  to  the  receipt  of  instructions.  Do  not  destroy  or  break  the 
seals  of  any  of  the  Seller's  No.  2  or  No.  3  samples  without  authori- 
zation from  the  General  Office. 

As  the  container  for  Seller's  No.  2  and  No.  3  samples,  use  a 
seamless  tin  salve  box  of  four  ounces  capacity,  provided  with  a 
slip  cover,  also  seamless.  Immediately  after  filling  seal  with  a 
double  layer  of  adhesive  tape,  to  exclude  moisture,  and  impregnate 
the  tape  with  at  least  two  coats  of  paraffin  by  rotating  the  box 
with  the  edge  immersed  in  melted  paraffin;  allow  each  coat  to  cool 
and  harden  before  applying  the  next  coat  which  is  used  to  close 
the  blowholes  in  the  previous  coat.  Attach  a  wax  seal  also  as  a 
guarantee  against  tampering. 

The  container  for  Seller's  No.  1  sample  may  be: 

(1)     A  seamless  tin  box  sealed  with  tape  and  paraffin  as 
described  above. 


*The  mill  should  be  of  the  size  which  has  a  jar  8.75  x  9.65  inches 
(outside)  rotating  at  the  rate  of  60-75  R.  P.  M. 


92  METHODS  OF  ANALYSIS 

(2)  A   glass   bottle  with   ground   glass  stopper,   sealed 
with  at  least  two  coats  of  paraffin. 

(3)  A  glass  bottle  with  a  flat  cork  stopper,  inserted  so 
that  the  top  of  the  stopper  is  at  least  %  inch  below 
the  top  of  the  neck  of  the  bottle,  and  covered  with  at 
least  two  coats  of  paraffin. 

3.  PREPARATION  OF  SAMPLE  FOR  ANALYSIS 

If  the  sample  has  been  prepared  as  in  2  (b),  no  further  prepa- 
ration is  required  before  analysis.  Otherwise  prepare  the  sample 
for  analysis  by  putting  the  entire  sample  through  a  sieve  having 
circular  openings  1  mm  in  diameter,  grinding  in  a  mortar  the 
portion  remaining  on  the  sieve  until  all  the  particles  pass  through. 
Grind  and  sift  as  rapidly  as  possible  to  prevent  absorption  of 
moisture,  and  avoid  exposing  any  of  the  material  unnecessarily  to 
the  air. 

4.     ANALYSIS  (GENERAL) 

Make  the  following  determinations  for  each  carload  shipped : 
moisture,  acid  insoluble,  lixiviated  ash,,  potash,  ammonia,  and 
screen  test.  Make  complete  analysis  of  a  composite  sample  repre- 
senting the  entire  season's  production. 

Use  due  care  in  weighing  on  account  of  the  hygroscopic  nature 
of  the  material.  Weigh  in  covered  dishes  or  watch  glasses,  or  from 
a  weighing  bottle,  and  as  a  rule  make  no  effort  to  secure  an  even 
fraction  or  multiple  of  a  gram. 

5.     MOISTURE 

Weigh  out  approximately  2  grams  in  a  covered  aluminum 
" moisture  dish."  Heat  for  about  5  hours  at  130°  C.,  cool  in  a 
desiccator  and  weigh.  Repeat  the  heating  for  one  hour  periods 
until  the  loss  of  weight  is  not  over  0.2%.  Consider  the  loss  in 
weight  to  represent  the  moisture. 

6.     ACID  INSOLUBLE. 

Weigh  out  approximately  1  gram,  transfer  to  a  250  ml  beaker, 
and  add  150  ml  of  water  and  15  ml  of  concentrated  hydrochloric 
acid.  Keep  the  beaker  covered  with  a  watch  glass  during  the 
addition  of  the  acid  and  add  the  acid  slowly.  Digest  on  a  hot  plate 
for  30—45  minutes.  Filter  through  a  tared  filter  or  Gooch  crucible 


X.      CRUDE  POTASH  93 

which  has  previously  been  washed  with  water  and  dried  to  constant 
weight.  Wash  with  hot  water,  and  dry  to  constant  weight  at 
100—105°. 

7.     WATER  INSOLUBLE 

Determine  as  in  "6,"  adding  water  but  no  hydrochloric  acid. 

8.     LIXIVIATED  ASH 

Weigh  out  approximately  1  gram  and  transfer  to  a  platinum 
dish.  Heat  to  a  dull  redness  to  carbonize  any  organic  matter 
present,  then  cool,  extract  with  water,  etc.,  following  the  procedure 
given  in  the  "General  Methods,  "  Chap.  I,  7  (b),  and  observing 
all  the  precautions  there  prescribed. 

9.     POTASH 
(*Lindo-Gladding  Method) 

REAGENTS 

(a)  Ammonium  Chloride  Solution:     Dissolve  100  grams  of 
ammonium  chloride  in  500  ml  of  water,  add  5  —  10  grams  of  pulver- 
ized potassium-platinic  chloride,  and  shake  at  intervals  for  6  —  8 
hours.     Allow  the  mixture  to  settle  over  night  and  filter.     The 
residue  may  be  used  for  the  preparation  of  a  fresh  supply. 

(b)  Platinum  Solution:    A  platinic  chloride  solution  contain- 
ing the  equivalent  of  1  gram  of  metallic  platinum  (2.65  grams  of 
H2PtCl6.6H20)  in  every  10  ml.     (Note  that  the  salt  sold  commer- 
cially as  "platinic  chloride"  has  the  formula  H2PtCl6.6H20). 

(c)  80%    Alcohol:      Grain    alcohol    of    sp.    gr.    0.8645    at 
C. 


DETERMINATION 

Boil  5  grams  of  the  sample  with  300  ml  of  water  for  thirty 
minutes.  Add  to  the  hot  solution  a  slight  excess  of  ammonium 
hydroxide  and  then  sufficient  ammonium  oxalate  (1  or  2  ml)  to 
precipitate  all  the  lime  present.  After  standing  for  one-half  hour, 
cool,  make  up  to  a  volume  of  500  ml,  mix,  and  pass  through  a  dry 
filter.  Evaporate  |25  ml  of  the  filtrate  nearly  to  dryness,  add 


*The  method  is,  with  a  few  additions  and  modifications,  that  of  the 
Association  of  Official  Agricultural  Chemists. 

tThe  pipette  and  flask  used  should  be  carefully  standardized  against 
each  other. 


94  METHODS  OP  ANALYSIS 

1  ml  of  dilute  sulphuric  acid  (1  to  1),  and  evaporate  to  dryness 
on  a  water  bath.  Finish  the  evaporation  on  a,  *Hillebrand  radiator 
and  ignite  until  all  ammonium  salts  are  expelled.  Maintain  a 
full  red  heat  until  the  residue  is  perfectly  white.  Dissolve  the 
residue  in  hot  water,  using  at  least  20  ml  for  each  decigram  of 
potassium  oxide  present.  Filter  if  there  is  any  insoluble  residue. 
Add  a  few  drops  of  hydrochloric  acid,  and  platinum  solution  in 
excess  (5  ml).  Evaporate  on  a  water  bath  to  a  thick  paste.  Treat 
the  residue  with  80%  alcohol,  avoiding  exposure  to  ammonia. 
Filter  through  a  Gooch  crucible  which  has  been  previously  washed 
with  80%  alcohol  and  dried  to  constant  weight.  Wash  the  pre- 
cipitate thoroughly  with  80%  alcohol  both  by  decantation  and  on 
the  filter,  continuing  the  washing  after  the  filtrate  is  colorless. 
Then  wash  with  10  ml  of  the  ammonium  chloride  solution  to 
remove  impurities  from  the  precipitate  and  repeat  5  or  6  times. 
Wash  again  thoroughly  with  80%  alcohol,  dry  the  precipitate 
for  30  minutes  at  100°  C.,  cool  in  a  desiccator,  and  weigh.  Repeat 
the  drying  until  constant  weight  is  attained.  The  precipitate 
should  be  perfectly  soluble  in  water.  Use  the  factor  .1938  to  con- 
vert K2PtCl6  to  K20. 

GOOCH  CRUCIBLES 

The  ignited  asbestos  for  the  felt  is  f prepared  as  follows :  Cut 
long-fibered  crysolite  asbestos  across  the  fibres  into  pieces  3/16  inch 
long,  and  ignite  in  a  crucible  or  dish  at  a  low  red  heat  for  at  least 
30  minutes.  When  cool,  transfer  to  a  porcelain  mortar  and  mace- 
rate to  a  pulp  with,  strong  hydrochloric  acid.  Dilute  this  paste 
with  a  large  amount  of  water,  pour  into  a  tall  beaker,  and  allow 
to  settle  until  the  fibrous  mass  collects  at  the  bottom,  leaving  the 
fine,  milky  silt  in  suspension.  Remove  all  of  this  fine,  milky  mate- 
rial by  repeated  washing  and  decantation  until  the  wash  water 
becomes  practically  clear.  Asbestos  prepared  in  this  manner 
makes  a  felt  that  filters  rapidly.  Preserve  in  water  in  a  stoppered 
bottle.  Form  the  filter  by  pouring  enough  of  the  suspended 
asbestos  into  the  crucible  to  form  a  layer  1/16  inch  thick  when 
drawn  down  by  suction.  Exactly  the  right  amount  must  be  learned 
by  experience.  A  properly  prepared  felt  will  filter  rapidly  and  yet 
retain  the  finest  precipitate.  Before  commencing  a  filtration, 
moisten  the  dry  filter  with  a  little  80%  alcohol. 


*Chap.  XXIII,  15. 

fBureau  of  Mines,  Technical  Paper  212,  p.  13. 


X.      CRUDE  POTASH  95 

10.     TOTAL  NITROGEN  AS  AMMONIA 

Determine  total  nitrogen  by  the  Kjeldahl  or  Gunning  method, 
both  modified  to  include  the  nitrogen  of  nitrates.  Calculate  the 
nitrogen  as  ammonia  (NH3). 

The  •Gunning1  Modified  Method  is  as  follows : 

REAGENTS 

For  ordinary  work  N/2  acid  is  recommended.  For  work  in 
determining  very  small  amounts  of  nitrogen  N/10  acid  is  recom- 
mended. In  titrating  mineral  acids  against  ammonium  hydroxide 
solution  use  cochineal  or  methyl  red  as  indicator. 

(a)  Standard    Sulphuric    Acid:      Determine    the    absolute 
strength  of  the  acid  by  precipitation  with  barium  chloride  solution 
as  follows:     Dilute  a  measured  quantity  of  the  acid  to  be  stand- 
ardized to  approximately  100  ml,  heat  to  boiling  and  add  drop  by 
drop  a  10%   solution  of  barium  chloride  until  no  further  pre- 
cipitation occurs.    Continue  the  boiling  for  about  5  minutes,  allow 
to  stand  for  5  hours  or  longer  in  a  warm  place,  pour  the  superna- 
tant liquid  on  a  tared  Gooch  or  on  an  ashless  filter,  treat  the  pre- 
cipitate with  25 — 30  ml  of  boiling  water,  transfer  to  the  filter  and 
wash  with  boiling  water  until  the  filtrate  is  free  from  chlorine. 
Dry,  ignite  over  a  Bunsen  burner  and  weigh  as  barium  sulphate. 
See  also  Chap.  XXV,  21  (a)   (3).    A  normal  solution  of  sulphuric 
acid  has  the  following  equivalents : 

1  ml  =  .04904  gram  H2S04 
1  ml  =  .01401  gram  N 
1  ml  =  .01703  gram  NH3 

(b)  Standard  Alkali  Solution:     Accurately   determine   the 
strength  of  this  solution  by  titration  against  the  standard  acid. 
N/10  solution  is  recommend. 

(c)  Sulphuric  Acid:   Of  sp.  gr.  1.84  and  free  from  nitrates 
and  ammonium  sulphate. 

(d)  Sodium  Hydroxide  Solution:    A  saturated  solution,  free 
from  nitrates. 

(e)  Cochineal  Solution:     Digest,  with  frequent  agitation,  3 
grams  of  pulverized  cochineal  in  a  mixture  of  50  ml  of  strong 
alcohol  and  200  ml  of  water  for  1  or  2  days  at  ordinary  tempera- 
ture, and  then  filter. 


*Methods  of  Anal,  of  the  Assoc.  of  Off.  Agric.  Chemists. 


96  METHODS  OF  ANALYSIS 

(f)  Methyl  Red  Solution:    Dissolve  1  gram  of  methyl  red 
(dimethyl-amino-azo-benzene-ortho-carbonic    acid)    in    100    ml    of 
95%  alcohol. 

(g)  Potassium  Sulphate:    Pulverized. 
(h)     Sodium  Thio sulphate. 

(i)     Commercial  Salicylic  Acid. 

APPARATUS 

(a)  Kjeldahl  Flasks  for   both   Digestion   and  Distillation: 
Total  capacity  of  about  550  ml,  made  of  hard,  moderately  thick, 
and  well-annealed  glass. 

(b)  Distillation  Flasks:     For  distillation  any  suitable  flask 
of  about  550  ml  capacity  may  be  used.     It  is  fitted  with  a  rubber 
stopper  through  which  passes  the  lower  end  of  a  Kjeldahl  con- 
necting bulb  to  prevent  sodium  hydroxide  being  carried  over  me- 
chanically during  distillation.     The  bulb  should  be  about  3  cm  in 
diameter,  and  the  tubes  should  be  of  the  same  diameter  as  the 
condenser  tube  with  which  the  upper  end  of  the  bulb  tube  is  con- 
nected by  means  of  rubber  tubing. 

DETERMINATION 

Place  0.7 — 3.5  grams,  according  to  the  nitrogen  content,  of  the 
substance  to  be  analyzed  in  a  digestion  flask.  Add  30 — 35  ml  of 
salicylic  acid  mixture  (30  ml  of  sulphuric  acid  to  1  gram  of  sali- 
cylic acid)  ;  shake  until  thoroughly  mixed,  and  allow  to  stand  for 
at  least  30  minutes  with  frequent  shaking.  Add  5  grams  of  sodium 
thiosulphatel  and  heat  the  solution  for  5  minutes;  cool;  add  10 
grams  of  potassium  sulphate  and  heat  very  gently  until  foaming 
ceases,  then  strongly  until  nearly  colorless.  Do  not  add  either 
potassium  permanganate  or  potassium  sulphide. 

After  cooling  dilute  with  about  200  ml  of  water.  Next  add 
sufficient  sodium  hydroxide  solution  to  make  the  reaction  strongly 
alkaline  (50  ml  is  usually  enough),  pouring  it  down  the  side  of 
the  flask  so  that  it  does  not  mix  at  once  with  the  acid  solution. 
Before  neutralizing  it  is  convenient  to  add  a  few  drops  of  phe- 
nolphthalein  indicator  or  a  piece  of  litmus  paper.  The  pink  color 
given  by  phenolphthalein  indicating  an  alkaline  reaction  is,  how- 
ever, destroyed  by  a  considerable  excess  of  strong  fixed  alkali. 

Connect  the  flask  immediately  with  the  condenser,  mix  the 
contents  by  shaking,  distil  into  a  measured  quantity  of  the  stand- 
ard acid  until  all  ammonia  has  passed  over,  and  titrate  with  the 


X.      CRUDE  POTASH  97 

standard  alkali.     The  first  150  ml  of  the  distillate  will  generally 
contain  all  the  ammonia. 

BLANKS 

Previous  to  use  the  reagents  should  be  tested  by  blank  experi- 
ments, and  correction  made  if  found  necessary. 

11.     SCREEN  TEST 

Weigh  out  500  grams  and  determine  the  percentage  retained 
by  a  12  and  20  mesh  sieve,  and  the  percentage  finer  than  20  mesh. 
Determine  the  percentage  of  the  finest  fraction  by  subtracting 
from  100.0  the  sum  of  the  percentages  of  the  other  fractions. 

Vary  this  test,  if  necessary,  to  suit  the  specifications  of  each 
sale  contract. 

12.     COMPLETE  ANALYSIS 

The  constituents  usually  reported  are  moisture,  acid  insoluble, 
potassium  chloride,  potassium  sulphate,  potassium  sulphide,  potas- 
sium carbonate  and  sodium  carbonate.  Directions  for  moisture, 
acid  insoluble,  and  potash  have  previously  been  given.  The  fol- 
lowing additional  determinations  are  required. 

(1)     TOTAL  ALKALI  AS  C02 

Extract  a  weighed  amount  with  hot,  neutral  water,  filter  and 
wash.  To  the  filtrate  add  a  few  drops  of  phenolphthalein  and  an 
excess  of  standard  sulphuric  acid.  Boil  until  all  of  the  carbon 
dioxide  has  been  expelled,  then  titrate  back  with  standard  sodium 
hydroxide. 

(2)     CHLORINE 

(*Volhard  Method) 
REAGENTS 

(a)  N/10  or  N/20  silver  nitrate. 

(b)  N/10  or  N/20  ammonium  or  potassium  sulphocyanate. 

(c)  Ferric  Indicator:    A  saturated  solution  of  ferric  alum 
(ferric  ammonium  sulphate). 

(d)  Nitric  Acid:     Free  from  lower  oxides  of  nitrogen,  se- 
cured by  diluting  the  usual  pure  acid  with  about  %  part  of  water, 
and  boiling  till  perfectly  colorless. 


*Methods  of  Anal,  of  the  Assoc.  of  Off.  Agric.  Chemists. 


98  METHODS  OP  ANALYSIS 

STANDARDIZATION 

Standardize  the  silver  nitrate  solution  by  titrating  in  the 
presence  of  nitric  acid  against  weighed  amounts  of  freshly  ignited 
C.  P.  sodium  chloride  (finely  powdered  and  heated  for  five  min- 
utes, not  quite  to  redness)  or  a  standard  solution  of  the  same. 
Standardize  the  sulphocyanate  solution  by  titrating  against  the 
silver  nitrate  solution.  Make  the  titrations  as  described  below 
under  * '  Determination. ' ' 

DETERMINATION 

Extract  a  weighed  amount  of  the  sample  with  50  ml  of  water 
in  a  200  ml  beaker.  Add  5  ml  of  colorless  nitric  acid  of  1.42  sp.  gr., 
heat,  filter,  and  wash  with  hot  water.  Add  about  2  ml  of  the  ferric 
indicator  to1  the  filtrate.  Then  add  a  few  drops  of  the  sulpho- 
cyanate solution  from  a  burette,  noting  the  quantity.  Titrate  with 
the  silver  nitrate  solution,  adding  it  drop  by  drop  and  stirring 
constantly,  to  decolorization.  Add  about  0.5  ml  more  of  the  silver 
nitrate  solution,  filter  off  the  silver  chloride,  and  wash  thoroughly 
with  hot  water.  Titrate  the  combined  filtrate  and  washings  to 
a  permanent  pink  color  with  the  sulphocyanate  solution.  Find  the 
amount  of  chlorine  by  difference  from  the  total  amounts  of  the 
silver  nitrate  and  sulphocyanate  solutions  used. 

(3)     SULPHURIC  ACID 

Dissolve  1  gram  of  the  sample  in  about  100  ml  of  water  and 
5  ml  of  concentrated  hydrochloric  acid,  in  a  flask  in  an  atmosphere 
of  carbon  dioxide.  Boil  the  hydrochloric  acid  solution,  main- 
taining the  atmosphere  of  carbon  dioxide,  until  any  hydrogen 
sulphide  evolved  is  completely  expelled.  Filter  and  wash  well 
with  hot  water.  Add  drop  by  drop  to  the  boiling  solution  an  excess 
of  hot  10%  barium  chloride  solution.  After  standing  over  night, 
filter,  wash  free  from  chlorine  with  hot  water,  ignite,  and  weigh 
as  barium  sulphate  (BaS04).  Add  a  drop  of  sulphuric  and 
hydrofluoric  acids  before  finishing  the  ignition;  this  will  remove 
any  silica,  if  present,  and  convert  any  reduced  barium  sulphide 
back  to  sulphate.  Multiply  the  weight  of  BaS04  by  .7465  to  con- 
vert to  K2S04. 

(4)     HYDROSULPHURIC  ACID 

Digest  1  gram  of  the  sample  with  about  100  ml  of  water,  and 
20  ml  of  bromine  water  to  oxidize  sulphides.  Acidify  with  hydro- 


X.      CRUDE  POTASH  99 

chloric  acid,  and  boil  to  complete  solution  and  expel  the  excess  of 
bromine.  Filter,  wash,  and  precipitate  the  sulphate  sulphur  in 
the  filtrate  with  barium  chloride  as  in  (3).  From  the  total  sulphur 
thus  determined,  expressed  as  "%  K2S04",  subtract  the  percent- 
age of  K,S04  found  in  (3),  and  multiply  the  difference  by  .6327 
to  obtain  the  percentage  of  potassium  sulphide  (K2S). 

(5)     HYPOTHETICAL  COMBINATIONS 

Calculate  all  of  the  chlorine,  sulphuric  acid,  and  hydrosul- 
phuric  acid  as  potassium  chloride,  potassium  sulphate,  and  potas- 
sium sulphide  respectively.  Calculate  the  remaining  potassium  as 
potassium  carbonate.  Subtract  the  C02  in  the  potassium  carbon- 
ate from  the  "  total  alkali  as  C02",  and  figure  the  remaining  C02 
as  sodium  carbonate. 


XI.     MOLASSES 

This  chapter  relates  to  the  sampling  and  testing  of  molasses 
in  storage  and  of  molasses  shipments.  Methods  relating  to  molasses 
in  connection  with  the  factory  process  or  the  Steffen  process  will 
be  found  in  an  appropriate  place. 

1.  STEFFEN  MOLASSES  BOUGHT  OR  SOLD 

Determine  on  every  car  on  the  top  sample : 

(a)  Brix. 

Determine  on  every  car  on  the  average  sample: 

(b)  Brix. 

(c)  Polarization. 

(d)  Apparent  Purity. 

SAMPLING 

Obtain  a  continuous  sample  through  a  small  tap  in  the  pipe 
line  while  each  car  is  being  loaded  or  unloaded.  After  the  car  is 
loaded,  or  before  it  is  unloaded,  take  another  sample  from  the  top 
of  the  car. 

ANALYSIS 

(a)  and  (b)  Brix:  Determine  by  the  double  dilution 
method,  I,  1  (b). 

(c)  Polarization:     Weigh  out  the  half -normal  weight  and 
determine  the  sugar  by  direct  polarization  as  in  Chap.  I,  3   (a). 

(d)  Apparent  Purity:    Follow  the  "General  Methods,"  I,  4. 

2.  DISCARD  MOLASSES  BOUGHT  OR  SOLD 

Determine  on  every  car  on  the  top  sample : 
(a)     Baume  at  100°  F. 


XI.      MOLASSES  101 

Determine  on  every  car  on  the  average  sample : 

(b)  Baume  at  100°  F. 

(c)  Polarization. 

SAMPLING 

Sample  in  the  same  manner  as  Steffen  molasses. 

ANALYSIS 

(a)  and  (b)  Baume  at  100°  F.:  Transfer  approximately 
one  quart  of  the  molasses  to  a  copper  vessel  about  6  inches  in  diam- 
eter by  8  inches  high.  Immerse  the  vessel  for  one  hour  in  a  *  water 
bath  to  such  an  extent  that  the  level  of  the  molasses  in  the  vessel 
is  below  that  of  the  water  in  the  bath,  and  keep  the  water  at  a 
gentle  boil,  or  within  a  few  degrees  of  the  boiling  point,  for  one 
hour.  Remove  any  foam,  fill  a  glass  cylinder  carefully  with  the 
molasses,  and  insert  a  thermometer.  Allow  the  molasses  to  cool, 
with  occasional  stirring.  When  the  temperature  has  fallen  to 
almost  100°  F.  (38°  C.),  insert  a  Baume  hydrometer  standardized 
as  described  in  Chap.  XXIV,  3  (d),  and  take  the  reading  at  exactly 
100°  F.  Be  sure  that  the  hydrometer  has  come  to  rest  before  the 
reading  is  made. 

(c)  Polarization:  Determine  as  in  the  case  of  Steffen 
molasses. 

3.    MOLASSES  IN  STORAGE 

SAMPLING 

Sample  each  molasses  storage  tank  once  a  week,  securing  one 
sample  from  the  top  and,  if  possible,  another  from  the  bottom. 

If  the  top  layer  contains  little  or  no  foam,  secure  the  sample 
by  dipping  three  inches  beneath  the  surface  with  an  ordinary 
sample  bucket.  If  foam  is  present,  use  a  suitable  sampling  device 
by  means  of  which  a  sample  of  the  molasses  immediately  beneath 
the  foam  may  be  obtained.  If  the  top  sample  shows  a  density  of 
less  than  42°  Baume,  take  additional  samples  at  gradually  increas- 
ing depths  to  determine  the  extent  of  this  condition. 

Secure  the  bottom  sample  from  the  pump  or  pipe  line,  or  from 
a  cock  located  near  the  bottom  of  the  tank. 

ANALYSIS 

Determine  the  "Baume  at  100°  F."  on  each  sample  according 
to  the  method  described  under  "2.  Discard  Molasses  Bought  or 
Sold." 


*This  is  for  the  purpose  of  removing  air  bubbles,  and  under  the  con* 
ditions  and  time  of  heating  specified  the  amount  of  evaporation  has  been 
found  to  be  unimportant. 


XII.  BEET  LABORATORY  TESTS 

1.  GENERAL 

The  purpose  of  the  beet  laboratory  tests  is  to  determine  the 
quality  of  the  beets  during  the  latter  part  of  the  growing  season 
and  at  the  time  of  delivery  during  the  harvest  season. 
Determine  on  each  sample: 

(a)  Sugar  by  Cold  Water  Digestion. 
Determine  as  often  as  required: 

(b)  Sugar  by  Hot  Water  Digestion. 

(c)  Apparent  Purity. 

As  beets  are  subject  to  both  evaporation  and  deterioration 
on  standing,  the  samples  should  be  worked  up  as  soon  after  receipt 
as  possible  and  should  not  be  allowed  to  accumulate. 

2.     PREPARATION  OF  SAMPLE 

As  each  sample  of  beets  is  brought  to  the  beet  laboratory  in 
a  sack  composed  of  such  material  as  will  best  prevent  evaporation, 
the  sample  should  not  be  removed  from  the  sack  until  shortly 
before  it  is  to  be  analyzed.  The  samples  should  be  cleaned,  if 
necessary,  and  freed  from  dirt  with  a  wire  brush  or  other  suitable 
apparatus,  avoiding  as  much  as  possible  injury  to  the  outside  sur- 
face. Delivery  samples  will  have  been  previously  tared  and  will 
require  no  cleaning  at  the  beet  laboratory.  Field  samples,  and 
sometimes  " piled"  samples,  will  require  cleaning. 

If  a  record  of  the  average  weight  is  desired,  count  and  weigh 
the  beets  constituting  the  sample,  and  enter  the  data  on  the  en- 
velope or  ticket  accompanying  the  sample. 

Reduce  a  segment  of  each  beet  of  the  sample  to  a  fine  pulp 
by  passing  the  beet  through  the  Keil-Dolle  rasp.  A  conical  rasp, 
such  as  the  Keil  disc,  has  been  found  by  us  by  careful  tests  to 


XH.      BEET  LABORATORY  TESTS  103 

take,  in  the  long  run,  an  average  sample  of  the  entire  beet,  but 
the  accuracy  of  the  sample  obtained  is  dependent  on  the  observa- 
tion of  the  following  points. 

(a)  Place  the  beet  in  position  firmly,  and  so  that  the  edge 
of  the  wedge  shaped  segment  removed  coincides  with  the 
axis  of  the  beet. 

(b)  Take  the   segment  from   the   first  beet  at  the  smaller 
diameter,  that  from  the  second  beet  at  the  larger  diam- 
eter, or  vice  versa,  and  so  on  alternately  with  the  re- 
maining beets  of  the  sample. 

(c)  See  that  all  the  beets  in  each  sample  are  rasped  and  that 
the  disc  and  pan  are  properly  cleaned  between  samples. 

The  reliability  of  the  cold  water  digestion  method  in  giving 
the  correct  percentage  of  sugar  depends  on  the  fineness  of  the 
pulp,  as  too  coarse  pulp  will  give  low  results  because  of  incomplete 
extraction  of  the  sugar.  The  production  of  sufficiently  fine  pulp  is 
dependent  on  the  observation  of  the  following  points. 

(d)  Push  each  beet  through  the  rasp  at  a  slow,  uniform 
rate  of  speed  which  has  been  found  by  experience  to 
give  pulp  of  the  proper  fineness.     The  operator  should 
never  be  allowed  to  force  the  beet  so  violently  against 
the  disc  as  to  retard  its  rotation  momentarily. 

(e)  See  that  the  rasp  is  always  up  to  the  required  speed 
of  600  revolutions  per  minute. 

(f)  Keep  the  rasp  in  proper  mechanical  condition,  as  de- 
scribed under  section  3,  "Care  of  the  Rasp." 

When  all  of  the  beets  of  the  sample  have  been  rasped,  clean 
the  disc  by  the  momentary  application  of  a  fiber  brush  to  each 
side.  Transfer  the  pulp  to  a  10  inch,  round  bottomed,  enameled 
mixing  bowl  by  means  of  a  metal  or  rubber  spatula  which  fits  the 
rasp  pan  closely.  Cover  the  bowl  if  the  balance  man  is  not  ready 
to  handle  the  sample  immediately. 

3.     CARE  OF  THE  RASP 

The  disc  must  be  mounted  on  the  shaft  so  that  the  edge  will 
run  true  without  oscillation.  New  discs  should  be  tested  to  see 
that  they  are  true,  as  otherwise  it  will  be  impossible  to  mount  them 
properly. 

The  disc  should  rotate  at  the  rate  of  600 — 700  revolutions  per 
minute. 


104  METHODS  OF  ANALYSIS 

The  ease  of  rasping  is  dependent  on  the  sharpness  of  the  teeth, 
but  the  fineness  of  the  pulp  is  dependent  on  an  even  contour  of  the 
edges  of  the  teeth.  If  a  rasp  is  found  to  give  too  coarse  pulp,  the 
disc  should  be  faced  by  holding  a  file  or  carborundum  stone  against 
both  the  sides  and  the  edge  of  the  rotating  disc.  Very  often  this 
procedure  can  be  improved  upon  by  first  going  over  the  disc  and 
filing  down  all  teeth  which  project  perceptibly  above  the  general 
contour;  large  side  teeth  close  to  the  edge  of  the  rasp  are  particu- 
larly objectionable  and  should  be  reduced  by  filing.  After  this 
treatment  very  little  facing  will  usually  be  necessary  to  put  the 
rasp  into  such  condition  that  it  will  produce  pulp  of  the  proper 
fineness.  The  facing  should  be  done  gradually  and  the  character 
of  the  pulp  tested  by  comparative  cold  and  hot  water  digestion, 
until  a  point  is  reached  where  the  rasp  yields  fine  pulp,  but  is  still 
sufficiently  sharp  so  that  the  beets  may  be  ground  without  undue 
effort.  New  discs  will  commonly  require  facing  before  the  pulp 
is  satisfactory.  The  quality  of  the  pulp  can  be  judged  only  ap- 
proximately, by  observation  and  must  be  determined  by  the  average 
difference  between  series  of  comparative  hot  and  cold  water  diges- 
tion tests.  This  difference  should  be  less  than  0.1  per  cent  on  the 
weight  of  the  beets,  and,  if  it  exceeds  this  figure,  the  rasp  should 
be  given  attention. 

When  the  disc  becomes  dull,  the  edge  teeth  should  be  shar- 
pened with  a  cant  file,  care  being  taken  to  keep  the  teeth  of  as 
uniform  size  and  even  contour  as  possible.  The  edge  should  then 
be  faced  lightly,  if  necessary,  as  previously  described.  As  the  edge 
becomes  wider  from  wearing  down,  it  will  be  found  increasingly 
difficult  to  obtain  fine  pulp,  until  a  point  is  eventually  reached 
where  the  disc  will  have  to  be  discarded. 

A  scale  of  calcium  oxalate  frequently  deposits  on  the  disc, 
especially  when  immature  beets  are  being  rasped.  As  this  forms 
a  polished  surface,  its  presence  is  easily  overlooked.  It  has  the 
effect  of  filling  up  the  interstices  between  the  teeth  and  thereby 
making  the  rasp  dull.  This  scale  can  be  removed  mechanically, 
or  very  readily  by  immersing  the  disc  in  strong  nitric  acid  diluted 
with  an  equal  volume  of  water.  The  scale  formation  will  be 
lessened  if  the  disc  is  washed  with  hot  water  whenever  the  rasp 
is  shut  down  for  any  length  of  time. 

The  rasp  pan  should  not  be  allowed  to  come  into  contact  with 
the  rotating  disc  when  it  is  removed  after  the  grinding  of  each 
sample.  For  the  same  reason  fiber  brushes  are  preferable  to  wire 
brushes  for  cleaning  the  discs  between  samples. 


XII.      BEET  LABORATORY  TESTS  105 

At  the  end  of  every  day  the  rasp  should  be  thoroughly  washed 
and  scrubbed,  and  then  dried  well. 

4.     DETERMINATION  OF  SUGAR  BY  COLD  WATER 
DIGESTION 

SPECIAL  APPARATUS 

(a)  A  pulp  balance  of  suitable  capacity  and  sensibility. 

(b)  A  sufficient  number  of  Monel  metal  capsules  about  3 
inches  high  by  3  inches  in  diameter,  all  adjusted  to  the  same  tare. 

(c)  Automatic  pipettes  which  have  been  carefully  standard- 
ized to  deliver  177  ml,  as  described  in  Chap.  XXIV,  2  (d). 

(d)  Aluminum  discs  with  a  round  hole  in  the  middle,  pro- 
vided with  rubber  envelopes,  to  serve  as  capsule  covers. 

SPECIAL  REAGENT 

(a)  Dilute  lead  acetate:  Mix  one  part  of  basic  lead  acetate 
solution  of  standard  strength  (55°  Brix)  with  30  parts  of  water. 
The  milky  solution  may  be  used  without  being  allowed  to  settle. 

DETERMINATION 

Mix  the  sample  of  fine  pulp  thoroughly  with  a  spoon  or 
spatula,  or  by  other  suitable  means.  Weigh  out  26  grams  in  a 
clean,  dry  capsule,  discarding  any  fragments  of  skin,  rootlets,  etc., 
which  may  be  occasionally  discovered.  Weigh  the  pulp  within 
an  accuracy  of  20  milligrams,  and  do  not  waste  time  in  attempting 
to  weigh  any  more  closely.  Add  177  ml  of  the  dilute  lead  acetate 
solution  from  the  automatic  pipette,  cover,  and  shake  vigorously 
for  a  few  seconds.  Let  the  covered  capsule  stand  for  at  least  20 
minutos,  again  shake  vigorously,  remove  the  cover,  filter,  and 
polarize  in  a  400  mm  continuous  tube.  The  reading  gives  directly 
the  percentage  of  sugar. 

Check  the  zero  point  of  the  polariscope  at  least  four  times  a 
day,  check  the  tare  of  the  capsules  once  a  day,  and  check  the 
normal  weight  frequently.  Check  the  thoroughness  of  the  mixing 
occasionally  by  making  sugar  determinations  on  several  samples 
taken  at  random  from  different  parts  of  the  same  bowl  of  pulp. 


106  METHODS  OF  ANALYSIS 

5.     DETERMINATION  OF  SUGAR  BY  HOT  WATER 
DIGESTION 

Check  the  accuracy  of  the  cold  water  digestion  tests  by  making 
hot  water  digestions  on  some  of  the  regular  samples  of  pulp.  In 
general  aim  to  check  about  5%  of  the  total  samples  in  this  way, 
and  in  particular  use  these  tests  to  keep  track  of  the  performance 
of  each  rasp  in  service.  The  average  difference  between  the  hot 
and  cold  water  tests  should  not  exceed  0.1%. 

Carry  out  the  hot  water  digestion  exactly  as  in  the  case  of 
cassettes,  as  described  in  Chap.  II,  1  (a),  with  the  following  modi- 
fication occasioned  by  the  fact  that  pulp  from  the  Keil-Dolle  rasp 
is  apt  to  contain  occluded  air  which  is  not  removed  by  ether  or  by 
prolonged  heating  during  digestion.  After  transferring  the  pulp 
to  the  200.6  ml  flask  and  adding  the  strong  lead  acetate,  fill  the 
flask  about  half  full  with  water  and  place  under  vacuum  for  3  or 
4  minutes,  carefully  at  first  until  frothing  has  ceased.  Then 
disengage  the  flask,  add  more  water,  and  proceed  with  the  digestion 
in  the  prescribed  manner. 

6.     APPARENT  PURITY. 

Make  up  a  composite  sample  by  taking  equal  portions  of  pulp 
from  a. number  of  the  regular  samples  after  rasping  and  mixing. 
Test  at  least  6  composite  samples  a  day,  and  make  it  a  rule  that 
each  composite  sample  shall  represent  the  same  number  of  indi- 
vidual samples,  in  order  that  a  correct  average  of  the  daily  work 
may  be  readily  obtained.  Do  not  hold  any  pulp  for  more  than  2 — 3 
hours,  however,  on  account  of  the  danger  of  deterioration. 

Obtain  the  pressed  juice  and  determine  the  apparent  purity 
exactly  as  described  in  Chap.  II,  1,  "Cassettes,"  under  "Prepara- 
tion of  Sample"  and  under  "Analysis,  (b)  Apparent  Purity," 
paying  due  regard  to  the  standard  pressure  specified. 


XIII.     ASH  ANALYSIS  OF  SUGAR  FACTORY  PRODUCTS 

1.     PREPARATION  AND  DETERMINATION  OF 
LIXIVIATED  ASH 

Weigh  out  approximately  3  grams  of  molasses  (in  the  case 
of  other  products  an  amount  equivalent  to  about  0.5  gram  of  ash) 
in  a  platinum  dish,  and  char  at  a  low  temperature,  never  employing 
a  full  red  heat  because  of  the  danger  of  volatilizing  alkali  chlorides 
and  of  fusing  the  ash.  Follow  exactly  the  procedure  for  the 
determination  of  lixiviated  ash  as  described  in  Chap.  I,  7  (b). 

It  will  probably  be  most  convenient  to  prepare  at  one  time 
sufficient  ash  for  all  the  determinations,  and  then,  after  grinding 
and  mixing,  preserve  it  in  a  tightly  stoppered  bottle.  Avoid  un- 
necessary exposure  to  the  air  in  preparing  the  sample,  so  that  it 
will  not  absorb  moisture.  As  the  anhydrous  ash  is  very  hygro- 
scopic, no  attempt  should  be  made  to  weigh  out  even  multiples 
or  fractions  of  a  gram;  weighing  by  difference,  from  a  weighing 
bottle,  is  recommended. 

To  save  time,  the  ash  used  for  the  determination  of  silica,  iron 
and  aluminum,  calcium,  and  magnesium ;  of  potassium  and  sodium ; 
and  of  phosphoric  acid  may  be  prepared  by  adding  sulphuric  acid 
to  a  weighed  amount  of  the  original  molasses  or  juice  in  each  case, 
and  igniting  as  in  the  determination  of  sulphated  ash,  I,  7  (a). 
In  this  case  the  percentages  of  the  various  constituents  must  be 
figured  on  the  percentage  of  lixiviated  ash  in  the  molasses  or  juice 
as  determined.  It  will  probably  be  preferable,  however,  to  use  a 
prepared  sample  of  lixiviated  ash  for  all  the  determinations,  as 
described  above. 

2.     SILICA  AND  INSOLUBLE 

Dissolve  approximately  0.5  gram  of  the  ash,  prepared  as  in 
"1,"  with  water,  cover  with  a  watch  glass,  and  add  cautiously 


108  METHODS  OF  ANALYSIS 

a  slight  excess  of  hydrochloric  acid.  Heat  till  effervescence  has 
ceased,  then  remove  and  wash  the  watch  glass,  and  evaporate  to 
dry  ness  on  the  water  bath.  Moisten  the  residue  with  5 — 10  ml  of 
concentrated  hydrochloric  acid,  cover  the  dish,  and  digest  for 
5 — 10  minutes  on  the  bath.  Add  sufficient  water  to  dissolve  the 
salts,  and  heat  again  on  the  bath  until  solution  is  complete.  Filter, 
wash  first  with  cold  water  or  with  hot  dilute  hydrochloric  acid,  and 
then  with  hot  water.  Evaporate  the  filtrate  to  dryness,  digest 
the  residue  with  acid  as  before,  but  in  smaller  amount,  and  repeat 
the  previous  procedure.  The  second  evaporation  will  usually  com- 
plete the  removal  of  all  the  silica.  Ignite  the  two  filters  over  a 
good  burner,  followed  by  a  blast  if  necessary,  and  weigh  as  Si(X. 

3.     IRON  AND  ALUMINUM 

(a)  In  the  absence  of  phosphoric  acid:    Oxidize  any  ferrous 
iron  in  the  filtrate  from  "2"  by  adding  several  milliliters  of  bro- 
mine water,  and  boil  off  the  bromine.     Then  cool  somewhat,  add 
enough  hydrochloric  acid  to  insure  a  total  of  10 — 15  ml  of  strong 
acid,  make  *slightly  alkaline  with  ammonium  hydroxide,  and  boil 
for  a  few  moments.    The  ammonia  should  not  be  in  such  excess  as 
to  require  long  boiling  to  expel  the  most  of  it,  nor  is  the  expulsion 
of  the  whole  of  it  necessary  or  desirable.     Filter  as  soon  as  the 
precipitate  settles,   wash  with   hot  water,   ignite,   and   weigh    as 
Fe203  +  A1203.    Multiply  by  .6994  to  obtain  the  iron  (Fe)  equiva- 
lent. 

(b)  In  the  presence  of  phosphoric  acid:    After  oxidizing  the 
iron  with  bromine  water  and  boiling  as  in  (a),  nearly  neutralize 
with  a  sodium  carbonate  solution,  adding  it  drop  by  drop  until 
a  slight  permanent  precipitate  is  produced,  which  is  then  redis- 
solved  by  the  addition  of  a  few  drops  of  hydrochloric  acid.     Add 
2 — 3  grams  of  sodium  acetate  (or  5 — 10  ml  of  a  30%  solution),  then 
add  a  ferric  chloride  solution  of  known  iron  content  drop  by  drop 
from  a  burette  as  long  as  any  precipitate  is  formed,  avoiding  any 
excess.    As  soon  as  the  phosphoric  acid  is  all  precipitated,  the  blood- 
red  ferric  acetate  is  formed.     If  the  solution  turns  red  without 
the  addition  of  any  ferric  chloride,  none  should  be  added,  for  in 
that  case  the  iron  is  in  excess  of  the  phosphoric  acid.     Up  to  this 
point  the  volume  should  be  kept  as  small  as  possible.    Now  dilute 
to  a  volume  of  at  least  150  ml  with  boiling  water,  and  boil  for 


*See  Hillebrand,  U.  S.  Geol.  Surv.  Bull.  700,  p.  107. 


XIII.      ASH  ANALYSIS  OF  SUGAR  FACTORY  PRODUCTS  109 

not  more  than  two  or  three  minutes.  Filter  while  hot,  and  wash 
with  hot  water  containing  a  little  sodium  acetate.  Redissolve  the 
precipitate  in  hydrochloric  acid,  using  enough  to  insure  a  total 
of  10 — 15  ml  of  strong  acid,  and  reprecipitate  with  ammonium 
hydroxide  as  in  (a),  combining  the  filtrate  with  the  filtrate  from 
the  basic  acetate  precipitation.  Ignite  and  weigh  as  Fe203  + 
A1203  -f-  PgOs-  From  the  weight  of  the  precipitate  deduct  the 
Fe203  equivalent  of  the  ferric  chloride  added,  deduct  also  the 
amount  of  P2O5  present  as  determined  in  "9,"  then  multiply  by 
.6994  to  obtain  the  iron  equivalent  of  the  iron  and  aluminum 
present. 

(c)  Determination  of  iron  and  aluminum  separately:  Fuse, 
in  a  platinum  crucible,  the  ignited  precipitate  obtained  as  in  (a) 
or  (b)  with  about  4  grams  of  fused  potassium  hydrogen  sulphate. 
This  fusion  takes  but  a  few  minutes  and  must  not  be  continued 
unnecessarily.  After  cooling,  add  5  ml  of  concentrated  sulphuric 
acid  and  heat  until  copious  fumes  of  sulphuric  acid  are  given  off. 
Cool,  transfer  to  a  flask,  add  water,  and  digest  till  the  solution  is 
clear.  Reduce  with  zinc,  cool,  titrate  with  N/50  potassium  per- 
manganate (standardized  against  sodium  oxalate),  and  calculate 
to  iron  (Fe).  Obtain  the  aluminum  by  difference. 

4.     CALCIUM 

Use  the  filtrate  from  3  (a),  or  the  two  combined  filtrates  from 
3  (b),  which  should  be  slightly  alkaline  with  ammonia.  To  the 
boiling  solution  add  drop  by  drop,  from  a  pipette,  burette,  or 
capillary  tube,  10  ml  of  hot  ammonium  oxalate  solution,  or  suf- 
ficient to  precipitate  all  the  calcium  present.  Filter  after  standing 
for  at  least  one  hour,  wash  with  hot  water,  and  determine  as  oxide 
or  sulphate  as  described  under  ''Limestone,"  Chap.  XVI,  5.  Mul- 
tiply the  weight  of  CaO  by  .7146,  or  of  CaS04  by  .2944,  to  convert 
to  calcium  (Ca). 

For  very  accurate  work,  the  ignited  calcium  oxide  is  dissolved 
in  hydrochloric  acid  and  reprecipitated  with  ammonia  and  ammo- 
nium oxalate. 

5.     MAGNESIUM 

To  the  filtrate  from  l<4"  add  10  ml  of  sodium  ammonium  phos- 
phate or  disodium  hydrogen  phosphate  solution.  After  vigorous 
stirring  add  ammonium  hydroxide  in  considerable  excess.  After 


110  METHODS  OF  ANALYSIS 

standing  over  night,  filter,  and  wash  with  dilute  ammonium 
hydroxide  (ammonium  hydroxide  of  0.90  sp.  gr.  diluted  to  ten 
times  its  volume).  Char  the  paper  slowly  without  allowing  it  to 
ignite,  burn  off  the  carbon  over  a  gradually  increasing  flame,  then 
apply  a  weak  blast  for  a  long  time  and  repeat  to  constant  weight 
to  insure  volatilization  of  any  excess  of  P205  over  and  above  that 
required  for  the  pyrophosphate  formula.  Weigh  as  Mg2P207  and 
multiply  by  .2184  to  convert  to  magnesium  (Mg). 

For  very  accurate  work,  the  precipitate  on  the  filter  is  dis- 
solved in  dilute  hydrochloric  acid,  and  the  magnesium  is  reprecipi- 
tated  by  adding  a  few  drops  of  sodium  or  sodium  ammonium  phos- 
phate and  ammonia,  which  is  added  gradually  with  stirring  and 
finally  in  slight  excess. 

6.    POTASSIUM  AND  SODIUM 

Extract  approximately  0.2  gram  of  ash,  prepared  as  in  "1," 
with  water  and  hydrochloric  acid  as  in  "2."  Remove  the  soluble 
silica  as  described  in  "  2, "  evaporate  the  filtrate  and  washings 
to  dryness,  dissolve  in  hot  water,  add  5  ml  of  barium  hydroxide 
solution,  and  heat  to  boiling;  let  settle  for  a  few  minutes,  and  de- 
termine if  the  precipitation  is  complete  by  the  addition  of  barium 
hydroxide  solution  to  a  little  of  the  clear  liquid.  When  no  fur- 
ther precipitate  is  produced,  filter  and  wash  thoroughly  with  hot 
water.  Heat  the  filtrate  to  boiling,  add  ammonium  hydroxide  and 
ammonium  carbonate  to  complete  the  precipitation  of  the  barium, 
calcium,  etc.,  let  stand  a  short  time  on  the  water  bath,  filter,  and  wash 
the  precipitate  throughly  with  hot  water;  evaporate  the  filtrate 
and  washings  to  dryness,  expel  ammonium  salts  by  heating  below 
redness,  treat  with  a  little  hot  water,  add  a  few  drops  of  ammonium 
hydroxide,  1  or  2  drops  of  ammonium  carbonate,  and  a  few  drops 
of  ammonium  oxalate ;  let  stand  a  few  minutes  on  the  water  bath, 
set  aside  for  a  few  hours,  filter,  evaporate  to  complete  dryness  on 
the  water  bath,  and  heat  to  dull  redness  until  all  ammonium  salts 
are  expelled  and  the  residue  is  nearly  or  quite  white.  Dissolve  in 
a  minimum  amount  of  water,  filter  into  a  tared  platinum  dish,  add 
a  few  drops  of  hydrochloric  acid,  evaporate  to  dryness  on  the 
water  bath,  heat  to  dull  redness,  cool  in  a  desiccator,  and  weigh 
as  potassium  and  sodium  chlorides.  Repeat  the  heating  until  con- 
stant weight  is  obtained.  Dissolve  in  a  small  amount  of  water; 
if  any  residue  remains,  the  separation  must  be  repeated  until  the 
residue  of  potassium  and  sodium  chlorides  is  entirely  soluble. 


Xni.   ASH  ANALYSIS  OP  SUGAR  FACTORY  PRODUCTS       111 

Dissolve  the  residue  with  water,  using  at  least  20  ml  for  each  deci- 
gram of  potassium  oxide  present,  add  5  ml  of  platinic  chloride 
solution,  and  proceed  as  in  the  determination  of  potash  by  the 
Lindo-Gladding  method,  Chap.  X,  9.  Calculate  the  sodium  by 
difference  from  the  weight  of  the  combined  potassium  and  sodium 
chlorides. 

If  the  determination  of  potassium  alone,  and  not  sodium,  is 
required,  this  may  be  made  by  saturating  the  original  juice  or 
molasses  with  sulphuric  acid,  and  proceeding  as  in  the  determina- 
tion of  potash  in  liquors  as  described  in  Chap.  IX,  12  (3). 

7.     CHLORINE 
(*Volhard  Method) 
REAGENTS 

(a)  N/10  or  N/20  silver  nitrate. 

(b)  N/10  or  N/20  ammonium  or  potassium  sulphocyanate. 

(c)  Ferric  indicator:     A  saturated  solution  of  ferric  alum 
(ferric  ammonium  sulphate). 

(d)  Nitric  Acid:     Free  from  lower  oxides  of  nitrogen,  se- 
cured by  diluting  the  usual  pure  acid  with  about  !/4  part  of  water, 
and  boiling  till  perfectly  colorless. 

STANDARDIZATION 

Standardize  the  silver  nitrate  solution  by  titrating  in  the  pres- 
ence of  nitric  acid  against  weighed  amounts  of  freshly  ignited  C.  P. 
sodium  chloride  (finely  powdered  and  heated  for  five  minutes, 
not  quite  to  redness)  or  a  standard  solution  of  the  same.  Stand- 
ardize the  sulphocyanate  solution  by  titrating  against  the  silver 
nitrate  solution.  Make  the  titrations  as  described  below  under 
' '  Determination. '  ' 

DETERMINATION 

Dissolve  a  weighed  amount  of  ash,  prepared  as  in  "1,"  in 
50  ml  of  water  in  a  200  ml  beaker.  Add  5  ml  of  colorless  nitric 
acid  of  1.42  sp.  gr.,  heat,  filter  if  there  is  any  important  amount 
of  insoluble  matter,  and  wash  with  hot  water.  Add  about  2  ml 
of  the  ferric  indicator  to  the  filtrate.  Then  add  a  few  drops  of 
the  sulphocyanate  solution  from  a  burette,  noting  the  quantity. 
Titrate  with  the  silver  nitrate  solution,  adding  it  drop  by  drop 
and  stirring  constantly  to  decolorization.  Add  about  0.5  ml  more 


*Methods  of  Anal,  of  the  Assoc.  of  Off.  Agric.  Chemists. 


112  METHODS  OF  ANALYSIS 

of  the  silver  nitrate  solution,  filter  off  the  silver  chloride,  and  wash 
thoroughly  with  hot  water.  Titrate  the  combined  filtrate  and 
washings  to  a  permanent  pink  color  with  the  sulphocyanate  solu- 
tion. Find  the  amount  of  chlorine  by  difference  from  the  total 
amounts  of  the  silver  nitrate  and  sulphocyanate  solutions  used. 

8.     SULPHURIC  ACID 

Extract  approximately  1  gram  of  ash,  prepared  as  in  "1," 
with  water  and  hydrochloric  acid  as  in  "2."  Filter,  wash  with 
hot  water,  heat  the  filtrate  to  boiling  and  add  drop  by  drop  5 — 10 
ml  of  a  hot,  10%  barium  chloride  solution,  or  sufficient  to  precipi- 
tate all  the  sulphuric  acid.  After  standing  over  night,  filter,  wash 
free  from  chlorine  with  hot  water,  ignite,  and  weigh  as  barium 
sulphate  (BaS04).  Add  a  drop  of  sulphuric  and  hydrofluoric 
acids  before  finishing  the  ignition;  this  will  remove  any  silica,  if 
present,  and  convert  any  reduced  barium  sulphide  back  to  sul- 
phate. Multiply  by  .4115  to  convert  to  S04. 

9.     ^PHOSPHORIC  ACID 

REAGENTS 

(a)  Moly~bdate  solution:     Dissolve   100  grams  of  molybdic 
acid    in    dilute    ammonium    hydroxide    (144    ml    of    ammonium 
hydroxide  of  0.90  sp.  gr.  and  271  ml  of  water)  ;  pour  this  solu- 
tion slowly  and  with  constant  stirring  into  dilute  nitric  acid  (489 
ml  of  nitric  acid  of  1.42  sp.  gr.  and  1148  ml  of  water.     Keep 
the  mixture  in  a  warm  place  for  several  days  or  until  a  portion 
heated  to  40°  deposits  no  yellow  precipitate  of  ammonium  phos- 
phomolybdate.      Decant    the    solution    from    any    sediment    and 
preserve  in  glass-stoppered  vessels. 

(b)  Ammonium  nitrate   solution:     Dissolve    200   grams   of 
commercial  ammonium  nitrate,  phosphate  free,  in  water  and  dilute 
to  2  liters. 

(c)  Magnesia  mixture:     Dissolve  22  grams  of  recently  ig- 
nited calcined  magnesia  in  dilute  hydrochloric  acid,  avoiding  an 
excess  of  the  latter.    Add  a  little  calcined  magnesia  in  excess,  and 
boil  a  few  minutes  to  precipitate  iron,  aluminum,  and  phosphoric 
acid;  filter;   add  280  grams  of  ammonium   chloride,   261   ml   of 
ammonium  hydroxide  (sp.  gr.  0.90)  and  dilute  to  2  liters.    Instead 
of  the  solution  of  22  grams  of  calcined  magnesia,  110  grams  of 
crystallized  magnesium  chloride  (MgCl2.6H20)  dissolved  in  water 


*Methods  of  Anal,  of  the  Assoc.  of  Off.  Agric.  Chemists. 


ASH  ANALYSIS  OF  SUGAR  FACTORY  PRODUCTS      113 

may   be  used,   then  add  280  grams  of  ammonium  chloride  and 
proceed  as  above. 

(d)  Dilute  ammonium  hydroxide  for  washing:  Dilute  100 
ml  of  ammonium  hydroxide  (sp.  gr.  0.90)  to  1  liter. 

DETERMINATION 

Extract  a  weighed  amount  of  ash,  prepared  as  in  "1,"  with 
water  and  hydrochloric  acid  as  in  "2."  Remove  the  soluble  silica 
as  described  in  "2,"  neutralize  the  filtrate  and  washings  with 
ammonium  hydroxide,  clear  with  a  few  drops  of  nitric  acid,  and 
add  about  15  grams  of  dry  ammonium  nitrate  or  a  solution  contain- 
ing that  amount.  To  the  hot  solution  add  60 — 80  ml  of  the  molyb- 
date  solution  for  every  decigram  of  phosphoric  acid  (P205)  that 
is  present.  Digest  at  about  65°  C.  for  an  hour,  and  determine  if 
the  phosphoric  acid  has  been  completely  precipitated  by  the  addi- 
tion of  more  molybdate  solution  to  the  clear  supernatant  liquid. 
Filter  and  wash  with  cold  water  or,  preferably,  ammonium  nitrate 
solution.  Dissolve  the  precipitate  on  the  filter  with  ammonium 
hydroxide  and  hot  water,  and  wash  into  a  beaker  to  a  bulk  of  not 
more  than  100  ml.  Nearly  neutralize  with  hydrochloric  acid,  cool, 
and  add  magnesia  mixture  from  a  burette;  add  slowly  (about  1 
drop  per  second)  stirring  vigorously.  After  15  minutes  add  12 
ml  of  ammonium  hydroxide  of  0.90  sp.  gr.  Let  stand  till  the 
supernatant  liquid  is  clear  (2  hours  is  usually  enough),  filter,  and 
wash  with  the  dilute  ammonium  hydroxide  until  the  washings 
are  practically  free  from  chlorine.  Ignite  the  precipitate  as  de- 
scribed under  the  determination  of  magnesium,  and  weigh  as 
magnesium  pyrophosphate,  Mg2P207.  Multiply  by  .6379  to  con- 
vert to  P205  and  by  .8534  to  convert  to  P04. 

10.     CARBONIC  ACID 

Carbonic  acid  (CO3)  is  usually  calculated  by  difference,  as 
the  amount  necessary  to  saturate  the  excess  of  basic  over  acid  ions. 
It  may  be  accurately  determined  by  the  method  described  in 
Chap.  XIV,  16. 

11.  HYPOTHETICAL  COMBINATIONS 
Join  phosphoric  acid  to  calcium;  if  there  is  any  uncombined 
phosphoric  acid  remaining,  join  it  to  magnesium  and  sodium  re- 
spectively. Then  assign  the  residual  basic  ions  in  the  following 
order:  potassium,  sodium,  magnesium,  calcium,  and  iron,  to  the 
residual  acid  ions  in  the  following  order :  chlorine,  sulphuric  acid, 
and  carbonic  acid. 


114  METHODS  OP  ANALYSIS 

Sometimes  the  total  of  all  the  constituents  or  the  direct  deter- 
mination of  carbon  dioxide  will  indicate  that  the  silica  should  be 
calculated  to  the  silicic  acid  ion  (Si03)  and  combined  with  calcium. 

12.     STATEMENT  OF  ANALYSIS 

Report  the  analysis  in  the  following  form: 

MOLASSES  ASH 

Factory.  (Date) 

Description  of  Sample: 

MOLASSES  ANALYSIS 

%  on        %  on  %  on 

Original  Dry  Sub.  Lix'd.  Ash 

Dry  Substance    80.12 

Lixiviated  Ash   11.46         14.30 

Sulphated  Ash    12.02         15.00 

Factor,  Sulph'd  to  Lix'd  Ash 953 

Potassium  Oxide,  K20 5.83  7.28  50.87 

Sodium  Oxide,  Na20   1.00  1.25  8.73 

%  on 

Lix'd  Ash 
ASH  ANALYSIS 

Silica  and  Insoluble 

Iron  and  Aluminum,  as  Iron Fe 

Calcium   .  Ca 

Magnesium    Mg 

Potassium    K 

Sodium Na 

Chlorine    Cl 

Sulphuric  Acid S04 

Phosphoric  Acid P04 

Carbonic  Acid C03 

Total   

COMBINATIONS 

Silica  and  Insoluble 

Potassium   Chloride    KC1 

Potassium  Sulphate K2S04 

Potassium  Carbonate K2C03 

Sodium  Carbonate  Na2C03 

Magnesium  Carbonate   MgC03 

Calcium  Carbonate   CaC03 

Ferrous  Carbonate FeCO3 

Sodium  Phosphate Na3P04 

Magnesium  Phosphate  .. .  .Mg3(P04)2 

Calcium  Phosphate    Ca3  (P04)  0 

Total   , 


(NOTE:     Omit  combinations  not  required.) 


XIV.     SCALES  AND  DEPOSITS 

The  composition,  of  scales  varies  so  widely  that  it  is  difficult 
to  prescribe  methods  for  everything  which  may  be  encountered. 
The  following  methods  will,  however,  generally  cover  the  impor- 
tant constituents  of  scales  deposited  from  water  or  juice  in  a 
beet  sugar  factory. 

1.     SAMPLING 

Obtain  samples  before  the  apparatus  is  boiled  out,  or,  if  this 
is  not  possible,  take  samples  after  boiling  out  and  include  a  nota- 
tion to  this  effect  in  the  record.  In  obtaining  the  sample  observe 
caution  to  avoid  contamination  with  the  underlying  metal.  To  this 
end  chipping  will  be  found  more  reliable  than  scraping.  Take  sam- 
ples from  several  parts  of  the  apparatus  in  which  the  scale  is  found, 
and  endeavor  in  every  case  to  get  portions  which  accurately  rep- 
resent the  entire  thickness  of  the  incrustation. 

Note  the  average  thickness  of  the  scale  (in  decimal  inches) 
using  calipers  where  practicable.  Note  also  the  hardness  and 
other  physical  characteristics  of  the  scale. 

2.     PREPARATION  OF  SAMPLE 

If  the  sample  is  moist,  dry  it  before  grinding.  Reduce  the 
entire  sample  to  60  mesh,  mix  thoroughly,  dry  20 — 50  grams  to. 
constant  weight  in  an  oven  at  100 — 105°,  cool  in  a  desiccator,  and 
preserve  in  a  stoppered  bottle.  From  this  one  general  sample 
take  all  weighed  portions  for  analysis. 

3.     QUALITATIVE  EXAMINATION 

Previous  to  any  quantitative  determinations,  examine  portions 
of  the  sample  for  the'  following :  insoluble,  soluble  silica,  copper, 
iron  and  aluminum,  manganese,  zinc,  calcium,  magnesium,  potas- 
sium, and  sodium;  and  for  the  following  acids:  hydrochloric, 
hydrosulphuric,  sulphurous,  sulphuric,  phosphoric,  carbonic,  oxalic. 


116  METHODS  OF  ANALYSIS 

acetic,  tartaric,  and  citric.    The  methods  for  the  qualitative  exam- 
ination are  so  well  known  that  they  need  not  be  repeated  here. 

Since  the  presence  of  manganese,  or  of  the  other  metals  not 
mentioned,  will  be  quite  unusual,  as  also  acetic,  tartaric,  and  citric 
acids,  the  quantitative  methods  for  them  will  not  be  given. 


QUANTITATIVE  EXAMINATION 
4.     INSOLUBLE 

Ignite  1  gram  of  the  thoroughly  dried  sample  in  a  platinum 
crucible  at  a  moderate  heat  to  decompose  organic  acids,  never 
heating  above  a  dull  redness,  on  account  of  the  danger  of  volatiliz- 
ing alkalies.  Transfer  to  a  beaker,  add  20  ml  of  1 :1  hydrochloric 
acid,  5 — 10  ml  of  concentrated  nitric  acid,  and  water  to  a  volume 
of  about  150  ml.  Digest  on  a  hot  plate  for  one  hour,  replacing 
the  water  lost  by  evaporation.  Filter,  wash  with  hot  water,  ignite 
and  weigh  the  residue. 

5.     SOLUBLE  SILICA 

Evaporate  the  filtrate  from  "4"  to  dryness  on  a  water  bath 
in  a  platinum  or  porcelain  dish.  Add  5 — 10  ml  of  concentrated 
hydrochloric  acid,  cover  the  dish,  and  digest  for  5 — 10  minutes  on 
the  bath.  Add  sufficient  water  to  dissolve  the  salts,  and  heat  again 
on  the  bath  until  solution  is  complete.  Filter,  wash  first  with 
cold  water  or  with  hot  dilute  hydrochloric  acid  until  the  absence 
of  any  yellow  color  in  the  precipitate  or  paper  indicates  the  re- 
moval of  the  iron,  then  finish  the  washing  with  hot  water.  Evapo- 
rate the  filtrate  to  dryness,  digest  the  residue  with  acid  as  before, 
but  in  smaller  amount,  and  repeat  the  previous  procedure.  The 
second  evaporation  will  usually  complete  the  removal  of  all  the 
silica.  Ignite  the  two  filters  over  a  good  burner,  followed  by  a 
blast  if  necessary,  and  weigh  as  Si02. 

6.     COPPER 

If  more  than  a  trace  of  copper  is  present,  remove  it  from  the 
filtrate  from  "5"  by  the  following  procedure.  Heat  the  solution, 
which  is  already  acid  with  hydrochloric  acid,  to  boiling,  and  satu- 
rate with  washed  hydrogen  sulphide  gas,  continuing  the  saturation 
until  the  solution  has  cooled  to  room  temperature.  Filter  off  the 
copper  sulphide,  washing  well  with  hydrogen  sulphide  water.  Do 


XIV.      SCALES  AND  DEPOSITS  117 

not  allow  the  filter  to  run  -  dry,  as  traces  of  the  sulphide  will  be 
oxidized  to  sulphate  on  exposure  to  the  air  and  will  pass  into  the 
filtrate. 

If  the  amount  of  copper  is  very  small,  it  may  be  estimated  with 
sufficient  accuracy  by  igniting  and  weighing  as  cupric  oxide 
(CuO).  Otherwise  use  the  following  volumetric  method. 

*Low  VOLUMETRIC  METHOD 

REAGENTS 

(a)  Standard  Sodium   Thiosulphate   Solution:     A  solution 
containing  19  grams  of  the  pure  crystals  in  1  liter. 

(b)  Starch  Indicator:    Mix  about  0.5  gram  of  finely  pow- 
dered potato  starch  with  cold  water  to  a  thin  paste;  pour  into 
about  100  ml  of  boiling  water. 

STANDARDIZATION 

Weigh  accurately  about  0.2  gram  of  pure  copper  foil  and 
transfer  to  a  250  ml  flask.  Dissolve  by  warming  with  5  ml  of  a 
mixture  of  equal  volumes  of  strong  nitric  acid  and  water.  Dilute 
to  50  ml,  boil  till  all  brown  oxides  of  nitrogen  have  been  expelled, 
add  5  ml  of  strong  bromine  water,  and  boil  until  the  bromine  is 
completely  driven  off.  Cool  somewhat  and  add  a  slight  excess 
of  strong  ammonium  hydroxide  (about  7  ml).  Again  boil  until 
the  excess  of  ammonia  is  expelled,  as  shown  by  a  change  of  color 
of  the  liquid  and  a  partial  precipitation.  Then  add  a  slight  excess 
of  strong  acetic  acid  (3  or  4  ml  of  80%  acid)  and  boil  for  a  minute. 
Cool  to  room  temperature  and  add  10  ml  of  30%  potassium  iodide 
solution.  Titrate  at  once  with  the  thiosulphate  solution  until  the 
brown  tinge  has  become  weak,  then  add  sufficient  starch  indicator 
to  produce  a  marked  blue  coloration.  Continue  the  titration 
cautiously  until  the  color  due  to  free  iodine  has  entirely  vanished. 
The  blue  color  changes  toward  the  end  to  a  faint  lilac.  If  at  this 
point  the  thiosulphate  be  added  drop  by  drop  and  a  little  time 
allowed  for  complete  reaction  after  each  addition,  there  is  no 
difficulty  in  determining  the  end  point  within  a  single  drop.  One 
ml  of  the  thiosulphate  will  be  found  to  correspond  to  about  0.005 
gram  of  copper. 

DETERMINATION 

Place  the  filter  containing  the  copper  sulphide  precipitate  in 
a  small  flask,  add  4 — 5  ml  of  concentrated  sulphuric  acid  and  the 


*Methods  of  Anal,  of  the  Assoc.  of  Off.  Agric.  Chemists. 


118  METHODS  OF  ANALYSIS 

same  amount  of  nitric  acid  and  heat  until  white  fumes  appear. 
Continue  the  oxidization,  adding  a  little  nitric  acid  from  time  to 
time,  until  the  liquid  remains  colorless  upon  heating  to  the  appear- 
ance of  white  fumes.  Cool,  dilute  with  about  30  ml  of  water,  add 
an  excess  of  bromine  water,  boil  until  all  bromine  is  expelled, 
and  proceed  exactly  as  above  under  ' '  Standardization. " 

7.     IRON  AND  ALUMINUM 

Boil  the  filtrate  from  "6"  to  expel  hydrogen  sulphide,  then 
add  bromine  water  (use  the  filtrate  from  "5"  if  copper  has  not 
been  determined)  and  proceed  as  in  Chap.  XIII,  3  (a)  or  (b), 
according  to  whether  phosphoric  acid  is  present  or  not.  Employ 
the  latter  method  (basic  acetate  separation)  in  any  case,  if  zinc 
is  to  be  subsequently  determined. 

8.    ZINC 

Having  precipitated  the  iron,  aluminum,  and  phosphoric  acid 
by  the  basic  acetate  method  as  in  Chap.  XIII,  3"  (b),  pass  hydrogen 
sulphide  into  the  filtrate  until  all  the  zinc  sulphide,  which  should 
be  pure  white,  is  precipitated.  Filter,  and  wash  with  hydrogen 
sulphide  water  containing  a  little  ammonium  nitrate.  Char  the 
paper  at  a  low  temperature,  heat  to  800 — 900°  in  a  muffle  for  one 
hour,  and  weigh  as  ZnO.  Multiply  by  .8034  to  convert  to 
zinc  (Zn.) 

9.     CALCIUM  AND  MAGNESIUM 

Boil  the  filtrate  from  "8"  to  expel  hydrogen  sulphide  (use 
the  filtrate  from  "7"  if  zinc  has  not  been  determined),  make 
alkaline  with  ammonia,  and  determine  as  in  Chap.  XIII,  4  and  5. 

10.  POTASSIUM  AND  SODIUM 
Determine  as  in  Chap.  XIII,  6,  or  as  follows: 
Weigh  out,  from  the  dried  sample,  enough  material  to  give 
approximately  0.2  gram  of  the  combined  sulphates  of  magnesium, 
potassium,  and  sodium.  Dissolve  in  hydrochloric  acid  and  remove 
silica  as  in  "4"  and  "5."  Concentrate  the  filtrate  and  add  a  few 
milliliters  of  dilute  sulphuric  acid.  Continue  the  evaporation  over 
a  Hillebrand  radiator  until  fumes  of  S03  come  off  copiously, 
repeating  the  addition  of  sulphuric  acid,  if  necessary,  to  decom- 
pose organic  matter.  Drive  off  the  excess  of  sulphuric  acid,  take 
up  with  hot  water  and  a  few  drops  of  hydrochloric  acid,  then 
remove  iron,  aluminum,  and  calcium  as  in  "7"  and  "9."  (This 


XIV.      SCALES  AND  DEPOSITS  119 

can  be  done  in  one  operation.)  Evaporate  the  filtrate  in  a  plati- 
num dish,  adding  toward  the  last  a  drop  or  two  of  sulphuric  acid, 
and  drive  off  the  ammonium  salts  and  the  last  traces  of  sulphuric 
acid  by  gentle  ignition.  Finally  heat  to  dull  redness,  preferably 
in  a  muffle,  to  decompose  bisulphates.  Cool  and  weigh  as  MgS04 
+  K2S04  +  Na,S04.  Repeat  the  ignition  to  constant  weight. 
From  this  point  on  avoid  exposure  to  ammonia  fumes. 

Dissolve  the  residue  in  water,  acidify  with  a  few  drops  of 
hydrochloric  acid,  add  chloroplatinic  acid  solution  in  excess  and 
proceed  as  in  the  determination  of  potassium,  Chap.  X,  8.  Mul- 
tiply the  weight  of  potassium  platinic  chloride,  converted  to  per- 
centage, by  .3854  to  convert  to  potassium  sulphate,  and  multiply 
the  percentage  of  magnesium,  determined  as  in  "8,"  by  4.9498  to 
convert  to  magnesium  sulphate.  Subtract  the  sum  of  these  two 
from  the  percentage  of  combined  sulphates  to  obtain  the  sodium 
sulphate,  which  multiplied  by  .3238  gives  the  percentage  of  sodium 
(Na)v.  Multiply  potassium  platinic  chloride  by  .1609  to  obtain 
potassium  (K). 

11.     CHLORINE. 

Determine  as  in  Chap.  XIII,  7.  It  sometimes  happens  that 
the  solution  is  too  dark  to  permit  the  chlorine  to  be  determined 
volumetrically.  In  this  event  proceed  as  follows: 

Prepare  a  nitric  acid  solution  of  a  weighed  portion  of  the 
material,  as  for  the  volumetric  method,  and  filter.  Add  a  sufficient 
amount  of  silver  nitrate  solution  to  precipitate  all  the  chlorine, 
avoiding  any  great  excess.  Heat  to  50°  and  allow  to  stand  for 
about  one  hour  in  a  dark  place.  Filter  through  a  Gooch  crucible, 
and  wash  the  precipitate  several  times  by  decantation  with  cold 
water  slightly  acidified  with  nitric  acid.  Transfer  the  precipitate 
to  the  Gooch  and  wash  free  from  silver  nitrate.  Dry  for  half  an 
hour  at  100°,  and  finally  at  130°  to  constant  weight.  Multiply 
silver  chloride  by  .2474  to  convert  to  chlorine  (Cl). 

12.  SULPHURIC  ACID  (SULPHATE  SULPHUR) 
(a)  Method  I:  Digest  1  gram  of  the  sample  with  about  100 
ml  of  water,  and  an  excess  of  bromine  water  or  sodium  peroxide 
to  oxidize  sulphides  and  sulphites.  Acidify  with  hydrochloric  acid, 
and  boil  to  complete  solution  and  expel  the  excess  of  bromine. 
Filter  and  wash  well  with  hot  water.  Add  drop  by  drop  to  the 
boiling  solution  an  excess  of  hot,  10%  barium  chloride  solution. 
After  standing  over  night,  filter,  wash  free  from  chlorine  with 


120  METHODS  OF  ANALYSIS 

hot  water,  ignite,  and  weigh  as  barium  sulphate.  Add  a  drop  of 
sulphuric  and  hydrofluoric  acids  before  finishing  the  ignition ;  this 
will  remove  any  silica,  if  present,  and  convert  any  reduced  barium 
sulphide  back  to  sulphate.  From  the  total  sulphur  thus  determined 
subtract  the  sulphite  and  sulphide  sulphur  determined  as  in  ' '  13 " 
and  "14"  to  obtain  the  sulphate  sulphur. 

(b)  Method  II:  Dissolve  1  gram  of  the  sample  in  about  100 
ml  of  water  and  5  ml-  of  concentrated  hydrochloric  acid,  in  a  flask 
in  an  atmosphere  of  carbon  dioxide.  Boil  the  hydrochloric  acid 
solution,  maintaining  the  atmosphere  of  carbon  dioxide,  until  the 
hydrosulphuric  and  sulphurous  acids  have  been  completely  ex- 
pelled. Filter,  wash,  and  precipitate  the  sulphate  sulphur  in  the 
filtrate  with  barium  chloride  as  in  Method  I.  Multiply  the  weight 
of  barium  sulphate  by  .4115  to  convert  to  S04. 

13.     SULPHUROUS  ACID   (SULPHITE  SULPHUR) 

APPARATUS 

A  distillation  flask,  set  above  a  burner,  and  fitted  with  a  3-hole 
rubber  stopper.  Through  one  hole  of  the  stopper  passes  a  dropping 
funnel  or  thistle  tube,  the  stem  of  which  reaches  nearly  to  the 
bottom  of  the  flask.  Through  another  hole  a  glass  tube  extends 
nearly  to  the  surface  of  the  liquid  in  the  flask  and  connects  at  the 
upper  end  to  a  carbon  dioxide  generator  through  a  washing  bottle. 
Through  the  third  hole  a  short  tube  leads  through  a  safety  bulb 
to  a  short  Liebig  condenser  which  is  so  inclined  that  the  lower 
end  reaches  well  into  the  receiving  vessel.  The  details  of  the 
generator  are  not  important  as  long  as  the  rate  of  flow  of  the  gas 
can  be  regulated  and  the  gas  passes  through  a  washing  bottle. 

DETERMINATION 

Transfer  10  grams  of  the  material  to  the  distillation  flask,  fit 
in  the  stopper,  and  connect  to  the  condenser  and  the  gas  gen- 
erator; then  introduce  through  the  funnel  or  thistle  tube  250  ml 
of  recently  boiled,  distilled  water..  Start  a  current  of  gas  through 
the  apparatus,  and  place  a  receiving  flask  or  beaker  containing 
100  ml  of  nearly  saturated  bromine  water  under  the  end  of  the 
condenser  with  the  tip  of  the  condenser  extending  below  the  surface 
of  the  bromine  water.  When  all  the  air  has  been  displaced  by 
carbon  dioxide  gas,  introduce  a  sufficient  amount  of  copper  sul- 
phate solution  to  prevent  the  distillation  of  sulphide  sulphur,  and 
add  10 — 20  ml  of  a  20%,  glacial  phosphoric  acid  solution,  intro- 


XIV.      SCALES  AND  DEPOSITS  121 

ducing  it  through  the  dropping  funnel  slowly  until  frothing  has 
ceased.  Start  the  distillation  and  continue  until  150  ml  of  dis- 
tillate has  passed  over,  watching  that  the  bromine  does  not  become 
too  weak  in  the  receiving  solution.  More  bromine  water  may  be 
added  from  time  to  time  if  necessary.  When  the  distillation  is 
completed,  disconnect  the  condenser  from  the  flask  and  rinse  with 
water  into  the  distillate.  Transfer  the  distillate  to  a  beaker,  boil 
off  the  excess  of  bromine,  add  5  ml  of  dilute  hydrochloric  acid 
(1  to  3),  and  precipitate  with  barium  chloride,  etc.,  as  in  "12." 
Multiply  the  weight  of  barium  sulphate  by  .3430  to  convert  to  S03. 

14.     HYDROSULPHURIC  ACID   (SULPHIDE  SULPHUR) 

% 

Determine  the  sulphide  sulphur  by  repeating  the  determina- 
tion for  sulphurous  acid  on  a  fresh  10  gram  sample,  following 
exactly  the  method  outlined  in  "12"  with  the  exception  that  no 
copper  sulphate  is  added.  By  this  procedure  the  hydrosulphuric 
acid  will  be  distilled  over  with  the  sulphurous  acid  and  be  weighed 
as  barium  sulphate.  Multiply  the  weight  of  barium  sulphate  thus 
found  by  .3430  to  convert  to  S03,  and  subtract  the  S03  determined 
as  in  "13"  to  obtain  the  S03  equivalent  of  the  sulphide  sulphur. 
Multiply  this  by  .4004  to  convert  to  sulphur  (S). 

15.    PHOSPHORIC  ACID 

Ignite  1  to  5  grams  of  the  sample  to  destroy  organic  matter, 
dissolve  in  dilute  hydrochloric  acid,  add  a  few  ml  of  nitric  acid, 
and  boil.  Then  remove  the  silica  and  proceed  as  in  Chap.  XIII,  9. 

16.     CARBONIC  ACID 

The  carbon  dioxide  in  the  carbonates  is  liberated  by  the  action 
of  dilute  sulphuric  acid,  purified  by  bubbling  through  a  mixture  of 
concentrated  sulphuric  and  chromic  acids,  and  caught  in  a  weighed 
potash  bulb. 

*APPARATUS 

A  wide  mouth  extractor  (C02)  flask  of  60  ml  capacity,  fitted 
with  a  3-hole  rubber  stopper  through  which  pass:  (1)  a  glass  tube 
leading  to  an  acid  reservoir;  (2)  a  connection  with  an  absorption 
tower  filled  with  soda-lime  to  remove  carbon  dioxide  from  the  air 
drawn  through  the  apparatus;  (3)  the  end  of  a  short  Liebig  reflux 


*An  illustration  of  a  suitable  arrangement  of  apparatus  is  given  on 
Page  104  of  W.  W.  Scott's  "Standard  Methods  of  Chemical  Analysis." 


122  METHODS  OP  ANALYSIS 

condenser  clamped  in  a  vertical  or  inclined  position.  The  second 
tube  should  extend  well  down  into  the  flask  so  that  the  incoming 
air  will  pass  directly  over  the  surface  of  the  liquid  in  the  flask. 
The  upper  end  of  the  condenser  is  connected  by  a  bent  tube  to  a 
bottle  of  sulphuric-chromic  acid  mixture,  through  which  the  gas 
bubbles  on  its  way  to  the  potash  bulb ;  this  serves  to  oxidize  S02 
and  H2S,  and  to  remove  the  moisture  in  the  gas  from  the  con- 
denser. A  calcium  chloride  tube  is  attached  to  the  potash  bulb  to 
catch  any  moisture  carried  over  from  the  potash  solution.  The 
exit  from  the  calcium  chloride  tube  is  connected,  through  a  guard 
tube  of  soda-lime  and  calcium  chloride  and  a  catchall  bottle,  to 
a  water  pump  which  serves  as  a  source  of  suction. 

The  Vanier  potash  bulb  is  preferable  to  the  older  Liebig  and 
Geissler  forms.  In  place  of  the  potash  bulb  may  be  used  a  pair 
of  soda-lime  U-tubes,  the  first  of  which  is  filled  with  soda-lime, 
while  the  second  is  filled  one-third  with  soda-lime,  followed  by 
calcium  chloride;  in  this  case  the  sulphuric  acid  bulb  serves  to 
indicate  the  rate  of  gas  flow. 

DETERMINATION 

Weigh  into  the  extractor  flask  a  portion  of  sufficient  size  to 
give  0.1 — .2  gram  of  C02,  fit  in  the  stopper,  connect  all  the  appa- 
ratus except  the  potash  bulb,  and  test  for  air  leaks.  Start  a  slow  cur- 
rent of  air  through  the  apparatus  by  means  of  the  suction  pump, 
and,  when  all  the  air  in  the  system  has  been  displaced  by  C02 — free 
air,  connect  the  potash  bulb,  which  has  been  previously  weighed. 
Thirty  minutes  should  be  ample  time  to  displace  the  air.  Then 
introduce,  very  slowly  at  first,  about  30  ml  of  10  per  cent  sulphuric 
acid  from  the  acid  reservoir.  Be  sure  that  the  acid  is  not  allowed 
to  liberate  so  much  carbon  dioxide  at  first  that  there  will  be  a 
backward  current  through  the  soda-lime  tower,  thereby  resulting 
in  the  loss  of  some  carbon  dioxide.  The  current  of  air  through 
the  apparatus  should  not  be  faster  than  a  safe  working  velocity 
for  the  type  of  potash  bulb  used.  When  all  the  acid  has  been 
introduced  boil  the  contents  of  the  flask  for  about  15  minutes  to 
expel  the  last  traces  of  carbon  dioxide,  remove  the  source  of  heat, 
and  let  the  air  current  continue  a  few  minutes  more,  then  discon- 
nect the  potash  bulb  and  weigh  it,  together  with  its  calcium  chloride 
tube.  The  increase  in  weight  gives  C02  directly,  and,  multiplied 
by  1.363'6,  the  equivalent  C03. 


XIV.      SCALES  AND  DEPOSITS  123 

Alternative  Method:  Employ  the  same  apparatus  and  man- 
ipulation as  just  described,  "but  in  place  of  the  potash  bulb  use 
three  small  bottles  filled  with  a  measured  amount  of  standard 
barium  hydroxide  solution.  See  W.  W.  Scott,  ''Standard  Methods 
of  Chemical  Analysis,"  page  107,  for  details. 

17.     OXALIC  ACID 
REAGENTS 

(a)  Calcium  <i<-<f<il<   xnlntion-:    A  5  to  10^   solution. 

(b)  N/10  potassium   permanganate:     Prepared   and   stand- 
ardized as  d<  scribed  in  Chap.  XVI,  9. 

DETERMINATION 

Method  I:  Transfer  1  gram  of  the  dried  sample  to  a  beaker, 
add  20  ml  of  1 :1  hydrochloric  acid  and  water  to  a  volume  of  about 
150  ml.  Digest  on  a  hot  plate  until  solution  is  complete,  filter,  and 
wash  with  hot  water.  Make  the  filtrate  slightly  alkaline  by  adding 
a  potassium  hydroxide  solution,  then  make  slightly  acid  with  acetic 
acid.  Heat  the  solution  to  boiling  and  add  slowly  a  hot  calcium 
acetate  solution  in  excess.  After  standing  over  night,  filter  and 
wash  the  precipitate  with  hot  water.  Determine  the  oxalic  acid 
by  dissolving  the  precipitate  in  dilute  sulphuric  acid  and  titrating 
with  permanganate  exactly  as  described  in  Chap.  XVI,  9. 

.17 '  thod  II:  Weigh  out  1  gram  of  the  dried  sample,  and  add 
10  grams  of  sodium  carbonate  and  75  ml  of  water.  Boil  for  about 
oO  minutes,  filter,  and  wash  with  hot  water.  Boil  the  residue  again 
with  2 — 3  grams  of  sodium  carbonate  and  a  small  amount  of  water, 
filter,  and  wash  with  hot  water.  Boil  with  sodium  carbonate  a  third 
time  in  the  same  manner;  the  third  extraction  will  complete  the  de- 
composition of  the  oxalates.  By  this  procedure  the  oxalic  acid 
will  all  be  found  in  the  filtrates  and  will  be  separated  from  the 
iron,  aluminum,  and  other  bases.  Make  the  combined  filtrates  acid 
with  acetic  acid,  heat  to  boiling,  and  proceed  as  in  Method  I,  above. 

18.     AMMONIA 

In  certain  scales  considerable  percentages  of  ammonia  will 
be  found.  Determine  by  distilling  with  strong  sodium  hydroxide 
into  standard,  acid  in  the  usual  manner  and  titrating  the  excess 
of  acid  with  standard  alkali,  using  cochineal  as  indicator.  No 
del  ailed  description  is  necessary  as  the  method  is  well  known. 


124  METHODS  OF  ANALYSIS 

19.     SUGAR 

Scales  formed  in  the  presence  of  saccharates  may  contain  con- 
siderable sugar.  Weigh  out  the  half-normal  weight  of  the  sample, 
rinse  into  a  50  ml  flask,  make  slightly  acid  with  acetic  acid,  add 
sufficient  basic  lead  acetate  solution  for  clarification,  and  dilute 
to  the  100  ml  mark.  Shake,  filter,  and  polarize.  The  reading  gives 
directly  the  percentage  of  sugar. 

20.     OIL 

Oil  will  be  found  in  many  sugar  factory  scales  and  is  deter- 
mined by  extraction  with  ether.  It  is  advantageous  to  make  the 
determination  on  a  dry  sample  which  has  been  lightly  ground  but 
not  pulverized,  owing  to  the  fact  that  a  fine  powder  containing  oil 
has  a  great  tendency  to  float  on  the  ether  and  be  carried  over  into 
the  extraction  flask. 

Wash  a  paper  thimble  with  ether,  dry  in  an  oven  at  100°,  and 
weigh  into  it  1  gram  of  the  sample.  Place  the  thimble  in  an  extrac- 
tion apparatus  and  extract  with  ether  until  extraction  is  complete. 
If  the  ether  is  free  from  sediment  or  suspended  matter  after  the 
extraction,  dry  the  thimble  as  before  and  weigh.  The  loss  in  weight 
represents  the  amount  of  oil.  If  particles  of  the  sample  have  been 
carried  over  into  the  extraction  flask,  instead  of  weighing  the 
thimble  filter  the  ether  solution  through  paper  and  evaporate  at 
40 — 50°,  weighing  the  residue  after  the  odor  of  ether  has  completely 
disappeared.  Evaporate  a  similar  volume  of  ether  to  determine 
the  necessary  correction  and  deduct  from  the  weight  of  the  residue. 
Call  the  difference  "oil." 

21.  GRAPHITE  AND  FREE  CARBON 

Finely  pulverize  the  dry  residue  from  the  oil  determination 
and  weigh  out  an  amount  equivalent  to  1  gram  of  the  original  dry 
sample,  treat  with  strong  nitric  acid  and  digest  until  the  evolution 
of  gas  ceases.  Repeat  this  nitric  acid  treatment  adding  a  little  con- 
centrated sulphuric  acid,  then  dilute  till  the  acid  is  not  too  strong, 
and  filter  on  an  asbestos  mat  in  a  Gooch.  Wash  successively  with 
a  little  water,  alcohol,  alcohol-ether  mixture,  alcohol,  hot  potas 
sium  hydroxide  solution,  hot  water,  dilute  hydrochloric  acid  and 
finally  with  hot  water.  (In  the  absence  of  carbonaceous  organic 
matter  the  washing  with  alcohol  and  ether  may  be  omitted.)  The 


XIV.      SCALES  AND  DEPOSITS  125 

n-sidiie  should  now  contain  only  graphite  and  free  carbon  and  pos- 
sibly some  silica. 

Dry  the  Gooch  and  its  contents  in  an  electric  muffle  at  180°  to 
constant  weight.  By  this  procedure  the  moisture  in  the  graphite 
and  free  carbon  will  be  driven  out  and  all  but  a  negligible  amount 
from  the  silica.  Cool  and  weigh.  Next  ignite  the  crucible  in  an 
electric  muffle  at  850°  to  950°  to  constant  weight.  Obtain  the 
graphite  and  free  carbon  together  by  difference. 

For  greater  accuracy  transfer  the  contents  of  the  Gooch  to  a 
decomposition  flask  and  determine  the  graphite  and  free  carbon 
I  iy  the  wet  combustion  method  for  the  determination  of  carbon, 
using  sulphuric  and  chromic  acids  and  weighing  the  carbon  dioxide 
absorbed  in  potassium  hydroxide.  For  details  of  the  method  con- 
sult Scott's  Standard  Methods  of  Chemical  Analysis,  pages  102 — 
103. 


XV.     COAL  AND  COKE 

1.     GENERAL 

Prepare  a  weekly  average  sample  of  the  coal  burned  during 
campaign  for  shipment  to  the  Central  Laboratory  in  accordance 
with  the  directions  in  Chap.  VII,  "Boiler  House  Control."  The 
Central  Laboratory  should  make  the  following  determinations : 
moisture,  volatile  matter,  fixed  carbon,  ash,  and  calorific  value. 

Analyze  a  sample  representing  each  car  of  coke  received, 
making  the  following  determinations :  moisture,  volatile  matter, 
fixed  carbon,  and  ash.  Determine  sulphur  on  a  composite  sample 
of  every  five  cars,  but  make  up  separate  composite  samples  for 
each  different  kind  of  coke. 

The  methods  of  analysis  are,  with  a  few  modifications,  *those 
of  the  U.  S.  Bureau  of  Mines. 

2.  SAMPLING  OF  COAL  AND  PREPARATION  OF  SAMPLE 

Directions  for  the  sampling  of  coal  burned  during  campaign 
will  be  found  in  Chap.  VII,  "Boiler  House  Control." 

Special  samples  may  be  required  at  times  for  carload  deliv- 
eries or  boiler  tests.  The  Bureau  of  Mines  recommends  a  gross 
sample  of  f  1,000  pounds  as  necessary,  whether  it  is  to  represent 
a  lot  of  1  ton  or  500  tons ;  a  gross  sample  of  $500  pounds  is  per- 
missible if  the  size  of  the  largest  piece  of  coal  or  impurities  is 
%  inch,  or  250  pounds  if  i/>  inch.  While  these  requirements  are 
not  usually  complied  with,  it  should  be  remembered  that  consid- 
erable variations  may  occur  in  the  analysis  to  the  extent  to  which 
the  size  of  the  gross  sample  is  below  the  figures  above  given. 

The  gross  sample  should  be  quickly  crushed  and  reduced  in 
acordance  with  the  ^methods  of  the  Bureau  of  Mines.  When  the 
sample  has  been  reduced  to  25  pounds,  or  if  the  gross  sample  does 
not  exceed  this  amount,  it  may  conveniently  be  ground  to  60  mesh 


*Bureau  of  Mines,  Technical  Papers  8  and  76. 

tBureau  of  Mines,  Bulletin  116,  pp.  13-15. 

{Bureau  of  Mines,  Bulletin  116,  p.  25,  and  Technical  Paper  133,  p.  9. 


XV.      COAL  AND  COKE  127 

si/.e  in  tin-  pebble  mill  described  in  Chap.  XXIII,  9.     About  6 
hours  is  required  for  grinding  _!•">  pounds. 

Smaller  samples,  which  have  to  be  ground  in  a  mortar  or  other 
apparatus  exposed  to  the  air,  should  first  be  air  dried  in  the  fol- 
lowing manner:  After  breaking  up  any  large  lumps,  place  the 
unground  sample  in  a  shallow  pan,  which  has  been  previously 

iied  and  is  a.irain  weighed  after  being  filled  with  the  coal. 
Kxpos»-  the  sample  to  the  atmosphere  of  the  room,  or  to  a  current 
of  air  raised  somewhat  above  the  ordinary  temperature  (30 — 35° 
C.),  until  two  successive  weighings,  made  6  to  12  hours  apart,  show 
a  loss  in  weight  of  not  over  0.2%.  (The  purpose  of  the  drying  is 
to  reduce  the  moisture  in  the  sample  to  such  an  extent  that  rapid 
change  in  weight  will  not  take  place  while  the  sample  is  being 
handled  in  the  course  of  analysis.)  Then  crush  the  sample,  reduce 
if  necessary,  and  grind  to  60  mesh.  Calculate  the  results  of  the 
analysis  to  coal  of  the  original  moisture  content. 

Any  samples  which  are  excessively  wet  should  be  air  dried, 
as  just  described,  before  being  ground. 

3.  SAMPLING  OF  COKE  AND  PREPARATION  OF  SAMPLE 

Approximately  75  small  pieces,  equivalent  to  a  total  weight  of 
1,000  to  1,500  grams,  obtained  by  being  broken  oft3  from  larger 
pieces  with  a  hammer,  should  be  taken  to  represent  as  nearly  as 
possible  an  average  of  the  car.  There  is  room  for  a  certain  amount 
of  personal  equation,  but  the  effort  should  be  made  to  obtain  as 
representative  a  sample  as  possible,  neither  intentionally  selecting 
nor  rejecting  any  coke  which  differs  in  appearance  from  the 
remainder. 

Reduce  the  75  pieces  constituting  the  original  sample  to  10 — 12 
mesh  si/e  with  a  jaw  cnisher.  If  a  crusher  is  not  available  use  a 
hammer,  but  crush  by  impact  with  the  avoidance  of  any  grinding. 
Mix  thoroughly,  being  careful  to  avoid  uneven  distribution  of  the 
fine  material  which  is  lower  in  ash  than  the  coarser  part,  and  grind 
15  grams  in  an  agate  mortar  to  pass  a  60  mesh  sieve;  to  avoid 
contamination,  reserve  a  60  mesh  sieve  for  this  purpose.  Mix  the 
ground  sample  well  and  transfer  it  to  a  stoppered  bottle. 

Do  not  use  bucking  boards,  disc  pulverizers,  or  any  kind  of 
mortar  except  an  agate  mortar  for  grinding  the  crushed  sample, 
on  account  of  the  danger  of  contamination. 


128  METHODS  OF  ANALYSIS 

4.    MOISTURE 

Weigh  out  1  gram  of  the  60  mesh  sample  in  a  covered  por- 
celain or  silica  *capsule  %  inch  deep  and  1%  inches  in  diameter, 
and  heat  for  exactly  one  hour  at  105°  in  a  constant  temperature 
oven.  The  Bureau  of  Mines  uses  an  oven  of  a  special  design 
through  which  a  current  of  dry,  preheated  air  is  passed.  It  will 
be  admissible  to  employ  a  glycerin  oven  of  the  regular  type  as 
described  in  Chap.  XXIII,  7,  without  the  use  of  an  air  current. 
Cool  the  covered  capsule  in  a  desiccator  over  sulphuric  acid  and 
weigh.  Call  the  loss  in  weight  "moisture  at  105°." 

Moisture  in  coke  can  also  be  determined  quickly  and  with 
adequate  accuracy  by  simply  heating  to  constant  weight  a  large 
sample  of  lump  coke,  in  any  convenient  oven,  or  on  a  stove,  hot 
plate,  or  steam  coil  at  a  temperature  of  100 — 200°  C. 

5.     ASH 

Determine  ash  in  the  same  sample  on  which  moisture  has  pre- 
viously been  determined.  Place  the  porcelain  capsule  containing 
the  sample  in  a  cool  muffle  and  raise  the  temperature  gradually 
to  about  750° ;  the  object  of  this  slow  heating  is  to  avoid  mechan- 
ical loss  from  the  rapid  escape  of  volatile  matter,  and  to  avoid 
coking  the  sample  and  thus  make  its  burning  difficult.  Continue 
the  ignition  in  the  muffle,  with  occasional  stirring  of  the  ash,  until 
all  particles  of  carbon  have  disappeared.  Cool  in  a  desiccator, 
weigh,  and  repeat  the  ignition  for  periods  of  half  an  hour  until 
the  difference  in  weight  between  two  successive  ignitions  is  less 
than  0.0005  gram.  In  the  absence  of  a  muffle,  ignite  over  a  flame, 
but  be  careful  first  to  drive  off  the  volatile  matter  slowly  at  a  low 
temperature. 

6.     VOLATILE  MATTER 

Employ  a  bright,  well  burnished,  10  ml  platinum  t crucible 
with  a  closely  fitting  capsule  cover;  the  crucible  should  be  1  inch 
in  diameter  at  the  top  and  1  3/16  inches  high,  and  the  crucible 
and  cover  together  should  weigh  about  15  grams.  Weigh  out  1 
gram  of  the  60  mesh  sample,  and  heat  for  4 — 6  minutes  over  a  low 
flame  in  order  to  avoid  mechanical  loss  from  the  rapid  escape 
of  steam  and  volatile  matter.  (This  preliminary  heating  is  neces- 
sary for  all  kinds  of  coal  analyzed  by  The  Great  Western  Sugar 

*Bureau  of  Mines,  Technical  Paper  76,  p.  16,  fig.  1,  a. 
fBureau  of  Mines,  Technical  Paper  76,  p.  18,  fig.  3,  a  and  b. 


XV.      COAL  AND  COKE  129 

Company,  and  for  petroleum  coke,  but  may  perhaps  be  dispensed 
with  in  the  case  of  coke  which  is  low  in  volatile  matter.) 

Follow  the  preliminary  heating  by  heating  for  exactly  7  min- 
utes in  an  electric  muffle  furnace  at  *850°.  Control  the  tempera- 
ture preferably  with  a  pyrometer.  Where  pyrometers  are  not 
available,  the  Central  Laboratory  will  furnish  standard  samples 
of  coal  and  coke  on  which  the  volatile  matter  has  been  determined 
at  850°  in  a  pyrometer-controlled  furnace.  The  temperature  of 
the  furnace  may  be  regulated  by  making  determinations  on  the 
standard  samples.  Seger  pyrometer  cones  may  also  be  found  useful. 

If  an  electric  furnace  is  not  available,  follow  the  preliminary 
heating  by  heating  for  exactly  7  minutes  on  a  platinum  or  nichrome 
triangle  in  the  full  flame  of  a  No.  3  Meker  or  Scimatco  burner. 
The  bottom  of  the  crucible  should  be  2  cm  above  the  top  of  the 
burner,  and,  to  protect  it  from  drafts,  it  should  be  enclosed  in 
a  sheet-iron  t chimney  of  special  design.  Adjust  the  height  of 
the  flame  so  that  the  temperature  in  the  interior  of  the  crucible 
will  be  850° ;  this  is  done  by  making  determinations  with  varying 
lengths  of  flame  on  the  standard  samples  furnished  by  the  Central 
Laboratory. 

After  heating  for  7  minutes  at  850°,  cool  in  a  desiccator  and 
weigh.  The  loss  in  weight  minus  the  weight  of  moisture  represents 
the  amount  of  "volatile  matter"  (at  850°). 

7.     FIXED  CARBON 

Subtract  from  100  the  sum  of  the  percentages  of  moisture, 
ash  and  volatile  matter. 

8.     SULPHUR 
REAGENT 

Eschka  Mixture  is  composed  of  two  parts  of  light  calcined 
magnesium  oxide  and  one  part  of  anhydrous  sodium  carbonate. 
It  may  be  purchased  in  the  form  of  an  analyzed  chemical. 

DETERMINATION 

Mix  1  gram  (or  for  convenience  of  calculation  1.373  grams) 
of  the  60  mesh  coal  with  6  grams  of  Eschka  Mixture  in  a  No.  1 


*The  Bureau  of  Mines  uses  a  temperature  of  950°.  This  temperature 
is  sometimes  difficult  to  reach  in  an  ordinary  electric  furnace  and  is  hard 
on  the  life  of  it.  The  temperature  adopted  in  any  case  is  a  matter  of 
arbitrary  selection. 

tBureau  of  Mines,  Technical  Paper  76,  p.  18,  fig.  3. 


130  METHODS  OF  ANALYSIS 

porcelain  crucible  and  heat  gradually  in  an  electric  muffle,  with 
free  access  of  air,  until  all  the  carbon  has  been  consumed.  If  an 
electric  muffle  is  not  available,  place  on  a  triangle  in  a  slanting 
position  and  burn  out  the  mixture  over  an  alcohol,  gasoline,  or 
natural  gas  flame ;  artificial  gas  as  a  rule  contains  so  much  sulphur 
that  its  use  may  introduce  an  error  in  the  determination.  Start 
tke  ignition  in  any  case  at  a  very  low  heat  to  avoid  driving  off 
volatile  matter  so  fast  that  unburned  sulphur  escapes ;  even  a  small 
loss  of  sulphur  dioxide  may  be  detected  by  its  pungent  odor.  The 
temperature  should  never  be  high  enough  to  cause  blackening  of 
the  top  of  the  Eschka  Mixture  in  the  crucible. 

After  the  crucible  has  been  heated  very  slowly  and  cautiously 
for  about  30  minutes,  increase  the  heat,  and  after  the  crucible 
becomes  red  hot  stir  the  contents  occasionally  until  all  black  par- 
ticles are  burned  out,  a  condition  which  indicates  that  the  reaction 
is  finished.  Cool,  transfer  the  crucible  with  its  contents  to  a  200 
ml  beaker,  and  digest  with  75  ml  of  hot  water  for  at  least  30 
minutes.  Filter  into  a»300  ml  beaker,  wash  the  insoluble  residue 
twice  with  hot  water  by  decantation  and  then  on  the  filter  'until 
the  volume  of  solution  in  the  300  ml  beaker  is  about  200  ml.  Add 
about  4  ml  of  saturated  bromine  water,  or  a  slight  excess,  and 
enough  concentrated  hydrochloric  acid  to  make  the  solution  slightly 
acid.  Boil  off  the  bromine  and  add  slowly  to  the  boiling  solution 
from  a  pipette  10  ml  of  a  hot  10%  barium  chloride  solution.  After 
standing  for  at  least  3  hours,  filter,  dry,  ignite,  and  weigh  as 
BaS04,  as  described  in  Chapter  I,  9.  To  obtain  the  percentage  of 
sulphur  multiply  the  weight  of  barium  sulphate  by  13.73  if  1  gram 
of  material  was  used,  or  by  10  if  1.373  grams  was  used.  • 


9.     CALORIFIC  VALUE 

Determine  the  heat  of  combustion  with  a  bomb  calorimeter, 
by  burning  one  gram  of  the  60  mesh  sample  in  compressed  oxygen 
gas  and  absorbing  the  total  heat  evolved  in  a  weighed  quantity 
of  water  in  which  the  bomb  is  immersed.  Measure  the  rise  in 
temperature  of  the  water  with  a  thermometer  that  is  graduated 
in  hundredths  of  1°  C.  and  can  be  read  by  a  telescope  to  .002°  C. 
Make  corrections  for  radiation,  combustion  of  the  iron  wire,  oxida- 
tion of  nitrogen  to  aqueous  nitric  acid,  and  oxidation  of  sulphur 
dioxide  to  aqueous  sulphuric  acid.  The  calorific  value  obtained 
in  this  manner  is  the  total  heat  of  combustion  with  water  vapor 


XV.      COAL  AND  COKE  131 

condensed  to  liquid  water  at  the  temperature  of  the  calorimeter, 
i.  e.,  20—25°  C. 

For  detailed  directions  consult  Technical  Paper  8  of  the 
Bureau  of  Mines  and  Circular  11  of  the  Bureau  of  Standards,  also 
the  pamphlet  of  directions  furnished  with  the  calorimeter.  On 
page  13  of  the  Bureau  of  Mines  Paper  is  given  an  explanation  and 
example  of  the  customary  method  of  calculating  the  radiation 
correction  ;  a  shorter  method  is  described  on  page  15  of  the  Bureau 
of  Standards  circular. 

The  correction  for  iron  wire  is  1.7  calories  (3.1  B.  T.  U.)  per 
milligram.  The  correction  for  sulphur  burned  to  sulphuric  acid 
is  13  calories  (23  B.  T.  U.)  per  0.01  gram  of  sulphur.  The  cor- 
rection for  nitrogen  to  aqueous  nitric  acid  is  made  by  titrating 
the  acidity  of  the  bomb  liquor  with  standard  ammonia  solution 
(0.00574  gram  NH3  per  ml),  using  methyl  orange  as  indicator, 
and  is  equivalent  to  5  calories  (9  B.  T.  U.)  per  milliliter.  These 
corrections  need  be  determined  only  occasionally  for  each  different 
type  of  coal. 

Use  only  thermometers  which  have  been  tested  by  the  Bureau 
of  Standards  and  make  the  necessary  corrections  according  to  the 
certificate.  The  thermometers  may  be  either  of  the  regular  kind 
with  a  scale  range  of  about  20 — 30°  C.,  or  of  the  Beckmann  or 
''differential'7  type.  Use  only  oxygen  which  is  made  by  a  liquid 
air  process;  do  not  use  electrolytic  oxygen,  which  contains  small 
amounts  of  hydrogen.  Check  the  water  equivalent  of  the  calori- 
meter by  burning  weighed  amounts  of  the  standard  "combustion 
samples"  (benzole  acid,  napthalene.  and  sucrose)  of  the  Bureau 
of  Standards  of  known  calorific  value. 


10.     ANALYSIS  OF  BOILER  HOUSE  ASHES 

See  Chap.  VII.  4  and  5,  regarding  the  sampling  of  boiler 
house  a-lies  and  the  preparation  of  the  samples. 

Dry  a  sufficient  amount  of  the  sample  to  approximately  con- 
stant weight  at  105°.  Determine  the  percentage  of  actual  ash  by 
igniting  1  gram,  or  approximately  this  amount,  of  the  dried  sample, 
as  described  in  the  determination  of  ash,  section  5  of  this  chapter. 
Figure  tlx-  percentage  of  ash  on  the  weight  of  the  dried  sample. 


132  METHODS  OF  ANALYSIS 

11.     BIBLIOGRAPHY 

"Methods  of  Sampling  Delivered  Coal"— Bur.  Mines,  Bulletin  116. 
"Directions  for  Sampling  Coal  for  Shipment  or  Delivery" — Bur. 

Mines,  Tech.  Paper  133. 
"Methods    of    Analyzing    Coal    and    Coke" — Bur.    Mines,    Tech. 

Paper  8. 
"Notes  on  the  Sampling  and  Analysis  of  Coal" — Bur.  Mines,  Tech. 

•Paper  76. 
"A    Convenient    Multiple-unit    Calorimeter    Installation" — Bur. 

Mines,  Tech.  Paper  91. 
"The   Determination   of  Moisture  in   Coke" — Bur.  Mines,    Tech. 

Paper  148. 
"The  Standardization  of  Bomb   Calorimeters" — Bur.   Standards, 

Circ.  11. 
"Standard     Samples — General     Information" — Bur.     Standards, 

Circ.  25. 
"Coal,"  by  E.  E.  Somermeier. 


XVI.     LIMESTONE 

1.     GENERAL 

Sample  every  car  of  limestone  and  determine  by  the  "rapid 
method :" 

(a)  Insoluble,   and  iron   and   aluminum   oxides    (together). 

(b)  Calcium  carbonate. 

At  the  end  of  every  week  make  up  a  composite  sample  repre- 
senting the  week's  deliveries  by  mixing  equal  portions  of  the  sam- 
ples of  the  individual  cars.  If  more  than  one  kind  of  limestone  has 
been  received,  make  up  and  analyze  separate  composite  samples 
for  each  kind.  On  the  weekly  average  samples  make  the  complete 
analysis  by  the  gravimetric  method,  determining : 

(a)  Insoluble. 

(b)  Iron  and  aluminum  oxides. 

(c)  Calcium  carbonate. 

(d)  Magnesium  carbonate. 

(e)  Calcium  sulphate,  if  present. 

Keep  the  individual  car  samples  for  at  least  two  weeks  before 
discarding,  for  possible  reference. 

2.  SAMPLING  AND  PREPARATION  OF  SAMPLE 

Approximately  75  small  pieces,  obtained  by  being  broken  off 
from  larger  pieces  with  a  hammer,  should  be  taken  as  uniformly 
as  possible  over  the  top  of  the  car  before  it  is  unloaded,  or  during 
the  unloading.  There  is  room  for  a  certain  amount  of  personal 
equation,  but  the  effort  should  be  made  to  obtain  as  representative 
a  sample  as  possible,  neither  intentionally  selecting  nor  rejecting 
any  stone  which  differs  in  appearance  from  the  remainder.  If  a 
piece  which  is  sampled  contains  a  coating  of  surface  material,  the 
small  sample  taken  should  be  broken  off  in  a  direction  which  will 
include  an  approximately  proportional  amount  of  this  surface 
material. 


134  METHODS  OF  ANALYSIS 

It  is  quite  essential  to  take  the  number  of  pieces  specified. 
Even  under  these  conditions  two  samples  from  the  same  car  taken 
by  different  operators  will  occasionally  differ  as  much  as  one  per 
cent  in  calcium  carbonate,  though  they  will  generally  be  much 
closer. 

Reduce  the  75  pieces  constituting  the  original  sample  to  ^4 
inch  size  with  a  jaw  crusher.  Mix  the  crushed  sample  well  and 
quarter  it.  Reduce  one  of  the  quarters  to  60  mesh  size  with  a  disc 
pulverizer.  Mix  the  finely  ground  sample  well,  and  preserve  a 
suitable  amount  in  a  stoppered  bottle. 


GRAVIMETRIC  METHOD 

3.     INSOLUBLE 

Dissolve  0.4 — .5  gram  in  50  ml  of  water  and  20  ml  of  concen- 
trated hydrochloric  acid,  in  a  beaker  covered  with  a  watch  glass. 
When  effervescence  has  ceased,  heat  to  boiling  and  digest  on  a  hot 
plate  for  10 — 15  minutes.  Filter,  wash  thoroughly  with  hot  water, 
ignite  and  weigh  the  "insoluble." 

4.     IRON  AND  ALUMINUM 

To  the  filtrate  from  "3"  add  several  milliliters  of  bromine 
water,  or  a  few  drops  of  concentrated  nitric  acid,  and  boil.  Then 
cool  somewhat,  make  slightly  alkaline  with  ammonium  hydroxide, 
and  boil  for  a  few  moments.  The  ammonia  should  not  be  in  such 
excess  as  to  require  long  boiling  to  expel  the  most  of  it,  nor  is  the 
expulsion  of  the  whole  of  it  necessary  or  desirable.  Filter  as  soon 
as  the  precipitate  settles,  wash  with  hot  water,  ignite,  and  weigh 
as  Fe203  +  Al,03. 

5.     CALCIUM 

Dilute  the  filtrate  from  "4"  to  a  volume  of  at  least  150  ml, 
heat  to  boiling,  and  to  the  boiling  solution  add  drop  by  drop,  from 
a  pipette,  burette,  or  capillary  tube,  20  ml  of  hot  ammonium 
oxalate  solution.  By  adding  the  reagent  in  this  manner  the  calcium 
oxalate  will  be  precipitated  in  a  granular  form  which  will  permit 
of  rapid  filtration  and  it  will  not  pass  through  the  filter  paper. 
Filter  after  standing  for  at  least  one  hour,  wash  two  or  three  times 
with  hot  water,  and  convert  to  oxide  or  sulphate,  as  described 
below. 


XVI.      LIMESTONE  135 

(a)  Determination  qs  Oxide:     Ignite  over  a  burner  of  the 
Meker  type  for  one-half  hour  or  longer,  in  a  platinum  crucible 
which  has  been  weighed  together  with  its  cover.    After  the  carbon 
is  all  burnt  off,  put  on  the  cover,  and  keep  the  crucible  covered 
during  the  balance  of  the  ignition,  and  during  cooling,  weighing, 
and  subsequent  ignitions.    Blast  for  successive  periods  of  5  minutes 
until  the  weight  is  constant,  or  heat  in  an  electric  furnace.     Cool 
in  a  desiccator  over  concentrated  sulphuric  acid,  which  should  be 
renewed  frequently,  especially  when  it  begins  to  show  any  sign 
of  discoloration,  and  do  not  let  the  crucible  stand  in  the  desiccator 
for  more  than  half  an  hour  before  weighing.     Weigh  as  calcium 
oxide,  and  multiply  by  1.7848  to  convert  to  calcium  carbonate 
(CaC03). 

(b)  Determination  as  Sulphate:     Ignite  in  a  platinum  cru- 
cible until  all  carbon  is  burnt  off,  but  not  necessarily  until  all 
carbonate  is  decomposed.     After  cooling,  slack  cautiously  with  a 
little  water  and  add  a  slight  excess  of  sulphuric  acid.     Evaporate 
on  a  *Hillebrand  radiator  until  all  the  free  acid  is  expelled,  heat 
to  dull  redness  over  a  flame,  and  weigh  as  calcium  sulphate.    Mul- 
tiply by  .7351  to  convert  to  calcium  carbonate. 

Sulphuric  acid  may  be  added  before  the  filter  paper  is  burnt, 
but  in  this  case  a  second  addition  of  sulphuric  acid  must  be  made 
after  tin-  carbon  is  all  burnt  off,  in  order  to  reconvert  any  sulphate 
reduced  to  sulphide  by  the  carbon  of  the  paper. 

When  calcium  is  weighed  as  the  sulphate,  certain  precautions 
are  necessary  as  calcium  sulphate  is  partially  converted  to  oxide 
at  a  red  heat.  After  the  final  addition  of  sulphuric  acid  the  cru- 
cible must  not  be  heated  above  a  dull  redness,  i.  e.,  a  redness  which 
is  barely  visible  in  daylight.  When  sulphuric  acid  is  added  before 
the  filter  paper  is  burnt  off,  this  degree  of  heat  must  not  be 
« 'X'-eeded  at  any  time  during  the  ignition.  After  weighing,  a  drop 
of  phenolphthalein  should  be  added;  if  the  precipitate  has  been 
properly  handled  it  should  not  give  a  pink  color  with  the  indicator. 
If  a  pink  color  is  produced,  add  a  little  sulphuric  acid  and  repeat 
the  previous  procedure  until  the  precipitate  fails  to  give  a  pink 
color  with  phenolphthalein. 

In  th<-  ignition  of  precipitates  in  general,  the  paper  is  most 
easily  burnt  if  high  temperatures  are  avoided,  especially  at  first. 
The  best  results  are  probably  obtained  by  charring  the  paper 
without  allowing  it  to  break  into  flame,  and  then  raising  the  tem- 


*See  Chap.  XXIII,  15. 


136  METHODS  OP  ANALYSIS 

perature  to  the  point  where  the  charred  residue  just  begins  to  glow 
nicely.  After  the  carbon  is  all  burnt  off,  the  crucible  may  be  raised 
to  whatever  temperature  the  conditions  of  the  particular  deter- 
mination require. 

6.    MAGNESIUM 

To  the  filtrate  from  "5"  add  10  ml  of  sodium  ammonium 
phosphate  or  disodium  hydrogen  phosphate  solution.  After  vig- 
orous stirring  add  ammonium  hydroxide  in  considerable  excess. 
After  standing  over  night,  filter,  and  wash  with  dilute  ammonium 
hydroxide  (ammonium  hydroxide  of  0.90  sp.  gr.  diluted  to  ten 
times  its  volume).  Char  the  paper  slowly  without  allowing  it  to 
ignite,  burn  off  the  carbon  over  a  gradually  increasing  flame,  then 
apply  a  weak  blast  for  a  long  time  and  repeat  to  constant  weight 
to  insure  volatilization  of  any  excess  of  P205  over  and  above  that 
required  for  the  pyrophosphate  formula.  Weigh  as  Mg2P207  and 
multiply  by  .7572  to  convert  to  magnesium  carbonate  (MgC03). 

7.     SULPHURIC  ACID 

Sulphur  seldom  occurs  in  important  amount  in  limestone  used 
by  beet  sugar  factories.  If  this  determination  is  necessary,  it  may 
be  made  as  follows :  Dissolve  1 — 2  grams  in  water  and  hydrochloric 
acid,  filter,  and  wash  with  hot  water.  Determine  the  sulphuric 
acid  in  the  filtrate  as  in  Chap.  XIII,  8.  If  sulphuric  acid  is  found 
present,  calculate  it  as  calcium  sulphate,  and  subtract  its  calcium 
carbonate  equivalent  from  the  calcium  carbonate  equivalent  of  the 
total  calcium  determined  as  in  "5-." 

Limestone  from  new  or  unfamiliar  quarries  should  always  be 
examined  for  sulphuric  acid. 

RAPID  METHOD 

8.     INSOLUBLE,  AND  IRON  AND  ALUMINUM  OXIDES 

Dissolve  0.4 — .5  gram  in  50  ml  of  water  and  20  ml  of  concen- 
trated hydrochloric  acid,  in  a  beaker  covered  with  a  watch  glass. 
When  effervescence  has  ceased,  heat  to  boiling  and  digest  on  a  hot 
plate  for  10 — 15  minutes.  Add  several  milliliters  of  bromine  water, 
or  a  few  drops  of  concentrated  nitric  acid,  and  boil.  Then  cool 
somewhat,  make  slightly  alkaline  with  ammonium  hydroxide,  and 
boil  for  a  few  moments.  Filter,  wash  well  with  hot  water,  ignite, 
and  weigh  as  ''insoluble"  +  Fe203  +  A1203. 


XVI.      LIMESTONE  1 37 

9.     CALCIUM 
RHAGBNT 

N/5  or  N/10  Potassium  rrrnunnfintate:  For  a  N/5  solution, 
dissolve  6.32  gnmis  of  the  pure  crystals  in  water,  filter  through 
asbestos,  and  make  up  to  1  liter.  One  ml  of  this  solution  will  be 
found  to  be  equivalent  to  about  .01  gram  of  calcium  carbonate. 
K.M  p  in  a  dark  bottle  well  protected  from  the  light.  The  solution 
should  be  allowed  to  stand  several  days,  if  possible,  before  it  is 
Mandardized,  and  its  value  will  vary  but  little  after  this  time.  As 
a  matter  of  precaution,  however,  it  is  well  to  restandardize  it  once 
a  month. 

STANDARDIZATION 

Weigh  out  1.34  grams  of  sodium  oxalate  of  the  *highest  purity 
obtainable,  dissolve  in  water,  add  50  ml  of  dilute  sulphuric  acid 
(1  to  10),  dilute  to  a  volume  of  about  150  ml,  heat  to  70°,  and 
titrate  to  a  permanent  pink  with  the  permanganate  solution.  From 
several  such  titrations  determine  the  calcium  carbonate  equivalent 
of  one  ml  of  the  permanganate. 

Sodium  oxalate  of  the  Bureau  of  Standards  may  be  used  for 
a  primary  standard.  Traces  of  moisture  can  be  removed  from 
sodium  oxalate  by  heating  at  120°  for  two  hours. 

DETERMINATION 

Dilute  the  filtrate  from  "8"  to"  a  volume  of  at  'least  150  ml, 
heat  to  boiling,  and  to  the  boiling  solution  add  drop  by  drop  from 
a  pipette,  burette,  or  capillary  tube,  20  ml  of  hot  ammonium 
oxalate  (4%  solution).  By  adding  the  reagent  in  this  manner 
the  calcium  oxalate  will  be  precipitated  in  a  granular  form  which 
will  permit  of  rapid  filtration  and  it  will  not  pass  through  the  filter 
paper.  Filter  after  standing  for  at  least  one-half  hour,  and  wash 
thoroughly,  but  not  excessively,  with  hot  water. 

Wash  the  precipitate  into  a  beaker  with  a  jet  of  hot  water, 
allowing  the  open  paper  to  cling  to  the  side  of  the  beaker  above 
tin-  liquid.  Add  50  ml  of  dilute  sulphuric  acid  (1  to  10),  pouring 
it  over  the  surface  of  the  paper.  Dilute  to  a  volume  of  about  150 
ml,  heat  to  70°,  and  titrate  with  the  permanganate  solution.  The 
reaction  requires  a  short  time  after  the  addition  of  the  perman- 
ganate, but,  after  it  once  begins,  the  permanganate  may  be  added 
quite  rapidly  until  the  end  point  is  nearly  reached.  Continue  the 


*Use  the  grade  "C.  P.  Special  for  Standardizing"  and  not  the  ordi- 
nary "C.  P." 


138  METHODS  OF  ANALYSIS 

titration  drop  by  drop  until  a  faint  pink  color  persists,  then  intro- 
duce the  filter  paper  and  add  a  few  drops  more  of  the  perman- 
ganate, if  necessary,  until  the  permanent  end  point  is  reached. 

10.     CARBONIC  ACID 

Ignite  0.5  gram  in  a  platinum  crucible  to  constant  weight  over 
a  good  burner,  followed  by  a  blast,  or  in  an  electric  furnace.  The 
loss  on  ignition  is  considered  to  represent  the  amount  of  carbon 
dioxide.  Check  the  efficiency  of  the  furnace  or  burner  occasionally 
by  the  ignition  of  pure  calcium  carbonate. 

If  moisture  is  present  in  the  original  sample,  it  must  first  be 
dried  for  one  hour  at  100 — 105°  and  then  weighed.  This  precaution 
is,  however,  hardly  ever  necessary. 

11.     CALCULATION  OF  RESULTS 

Multiply  the  percentage  of  C02  (loss  on  ignition)  by  2.2742  to 
obtain  the  percentage  of  total  carbonates  as  calcium  carbonate. 
Subtract  the  percentage  of  calcium  carbonate,  as  determined  in 
"9,"  and  multiply  the  difference  by  .8426  to  obtain  the  percentage 
of  magnesium  carbonate. 


XVII.     WATER 

1.     SAMPLING  OF  WATER  FOR  BACTERIOLOGICAL 
EXAMINATION 

(a)  APPARATUS 

Use  sterilized  bottles  provided  with  glass  stoppers  and  with 
cloth  caps  secured  by  a  rubber  band.  The  bottles  are  cleansed 
with  great  care,  rinsed  in  clean  water,  and  sterilized,  together  with 
the  stoppers  and  caps,  by  heating  to  180 — 190°  C.  A  suitable  ship- 
ping case,  containing  compartments  for  the  bottles  and  for  icing, 
is  also  required. 

(b)  PROCEDURE 

Adhere  strictly  to  the  following  procedure : 

(1)  Allow  a  good  stream  to  run  from  the  faucet  or  source 
of  supply  for  at  least  10  minutes  before  the  sample  is  taken,  in 
order  that  one  may  be  sure  of  obtaining  fresh  water  and  not  water 
which  has  been  standing  in  the  pipe. 

(2)  Remove  the  rubber  band  and  the  cloth   cap   from  the 
bottle,  being  careful  not  to  drop  the  cap  or  to  allow  anything  to 
touch  the  inside  of  it. 

(31)  Rinse  the  outside  of  the  bottle,  with  the  stopper  in  place, 
with  water  from  the  source  of  supply  which  is  to  be  sampled. 

(4)  Remove  the  stopper,  being  careful  not  to  touch  any  part 
of  it  except  the  portion  which  projects  outside  the  bottle. 

(5)  Fill  the  bottle  completely  with  the  water  to  be  tested. 

(6)  Holding  the  bottle  in  one  hand  and  the  stopper,  in  an 
inverted  position,  in  the  other  hand,  invert  the  bottle  and  allow 
some  of  the  water  to  run  out  over  the  stopper.    Insert  the  stopper 
while  pouring,  thus  leaving  some  air  space  to  allow  the  bottle  to 
!•••  shaken  before  plating. 

(7)  Rinse  the  outside  of  the  bottle  again. 


140  METHODS  OF  ANALYSIS 

(8)  Put  the  cap  on  the  bottle,  and  secure  with  the  rubber 
band. 

(9)  Label  the  bottle  with  regard  to  the  source  of  sample,  time 
when  taken,  etc. 

Observe  care  to  omit  none  of  the  steps  in  the  procedure  above 
described.  Number  Seven,  which  calls  for  rinsing  the  stopper  and 
the  outside  of  the  bottle  after  the  stopper  has  been  inserted,  is 
probably  the  one  which  is  most  apt  to  be  forgotten. 

Immediately  after  the  samples  have  been  taken,  ship  them 
on  ice  to  the  laboratory  where  they  are  to  be  tested. 

2.     SAMPLING    OF    WATER   FOR    CHEMICAL   ANALYSIS 

No  particular  directions  are  needed  with  regard  to  the  collec- 
tion of  special  samples.  The  following  instructions  relate  to  the 
collection  of  weekly  and  campaign  average  samples  for  analysis: 

(a)     CAMPAIGN  AVERAGE  SAMPLES 

A  composite  sample  of  each  kind  of  water  of  importance,  as 
described  below,  should  be  made  up  during  the  campaign  and 
analyzed  after  the  end  of  the  campaign.  The  Chief  or  Assistant 
Chemist  should  once  a  shift  obtain  the  required  samples,  and,  in 
order  to  avoid  contamination  with  sulphuric  acid,  he  should  use 
a  different  set  of  test  tubes;  or  receptacles  from  that  used  by  the 
sample  carrier  who  obtains  samples  for  the  alpha-naphthol  tests. 
A  measured  volume  of  each  kind  of  water  should  be  transferred 
to  a  bottle  of  suitable  size,  'appropriately  labeled,  to  form  the 
composite  sample.  Sufficient  water  should  be  taken  so  that  the  final 
volume  will  amount  to  at  least  2  liters,  and  preferably  more  in 
the  case  of  waters  low  in  solids.  It  is  advisable  to  make  up  several 
composite  samples  of  each  water,  representing  successive  periods 
of  three  or  four  weeks  each  during  the  campaign,  and  to  test  these 
for  contamination  before '  mixing  to  form  the  general  composite 
sample. 

The  collection  of  these  samples  should  be  started  as  soon  after 
the  beginning  of  the  campaign  as  possible,  when  it  is  certain  that 
the  waters  are  running  in  a  normal  manner.  Samples  should  be 
taken  of  all  "condensed  water,"  "main  supply  waters,"  etc.,  and 
will  include  the  following: 

"Water  from  Boiler  Feed  Tank 

Condensed  Water  Pumped  Direct  to  Boilers 

Water  in  Boilers 


XVII.      WATER  141 

Water  Used  for  Washing  Hot  Presses  and  Saccharate  Presses 

Pure  Battery  Supply  Water 

Impure  Battery  Supply  Water 

All  Condensed  Waters  (including  all  that  are  tested  regularly) 

All  Main  Supply  Wraters,  such  as  Ditch,  Well,  River,  and  City 

Water 

All  Cooling  Waters,  including  Tail  Pipe  Waters 
In  addition  to  the  above,  any  waters  that  may  be  necessary  to 

complete  the  record. 

Analyses  of  different  samples  representing  the  same  water 
need  not  be  unnecessarily  duplicated.  Thus  if  all  or  a  number 
of  the  pan  condensers  are  supplied  with  the  same  water,  a  single 
composite  sample  may  be  made  up  for  analysis  from  the  composites 
of  the  individual  tail  pipes.  Separate  samples  should  be  saved, 
however,  so  that  they  will  be  available  if  any  change  is  made  in 
the  water  system  during  the  campaign. 

(b)  WEEKLY  AVERAGE  SAMPLES  OF  BATTERY  SUPPLY  WATER 
\\Vekly  composite  samples  of  the  battery  supply  water  should 

also  be  collected  in  the  same  manner  as  the  campaign  average 
samples,  separate  samples  of  the  "pure"  and  "impure"  water 
being  taken  if  a  dual  system  is  in  use.  At  the  end  of  every  week 
filter  the  water  and  determine  the  total  solids,  as  described  below. 

(c)  AVERAGE  SAMPLES  DURING  POTASH  CAMPAIGN 

Factories  engaged  in  potash  recovery  should  also  collect  aver- 
age samples  for  the  potash  campaign  of  all  waters  sampled  for  the 
same  purpose  during  the  beet  campaign,  as  described  in  (a)  above, 
and  in  addition  should  obtain  average  samples  of  the  condensed 
water  from  the  steam  chamber  of  each  evaporator  body.  These 
samples  should  be  analyzed  in  full,  and,  in  any  water  which  may 
be  contaminated  with  potash  liquors  by  leaks  or  entrainment. 
potassium  should  be  determined  separately  as  described  in  Chap. 
XIV,  10. 

ANALYSIS 

The  methods  are  taken  from  various  sources,  following  in  many 
cases  those  of  the  Association  of  Official  Agricultural  Chemists. 
Make  all  determinations  on  water  which  has  been  freed  from  sus- 
pended matter  by  filtration. 


142  METHODS  OF  ANALYSIS 

3.     TOTAL  SOLIDS 

Allow  the  sample  to  stand  until  all  sediment  has  settled,  and 
filter  if  necessary  to  secure  a  perfectly  clear  liquid.  Evaporate 
*500  ml  (preferably  more  if  the  water  is  low  in  solids)  in  a  weighed 
platinum  dish  on  a  water  bath.  Additional  platinum  and  porcelain 
dishes  may  be  used  to  hasten  the  evaporation,  the  various  concen- 
trated portions  being  finally  rinsed  into  the  weighed  platinum 
dish,  with  the  aid  of  a  "policeman"  to  remove  crystallized  salts. 
After  evaporation  to  dryness,  heat  to  constant  weight  at  105°  C. 
in  a  constant  temperature  oven. 

Where  the  complete  analysis  is  not  required  and  the  deter- 
mination of  total  solids  alone  is  necessary,  as  in  the  case  of  the 
weekly  samples  of  battery  supply  water,  evaporate  100  ml  as  above, 
and  dry  at  i05°  C. 

4.     TOTAL  SULPHATES 

Dissolve  the  residue  from  "3"  in  the  least  possible  amount  of 
distilled  water,  and  acidify  with  3-5  ml  of  dilute  sulphuric  acid 
(1:10).  Evaporate  first  on  the  water  bath,  and  then  carefully  at 
a  ftemperature  sufficiently  high  to  expel  the  excess  of  sulphuric 
acid  without  loss.  Heat  finally  to  a  redness  which  is  barely  visible 
in  daylight  until  the  residue  is  white ;  cool,  and  weigh. 

This  treatment  is  prescribed  to  destroy  organic  matter,  and 
for  the  indirect  determination  of  the  sodium.  Subtract  from  the 
weight  of  "total  sulphates"  the  amount  of  calcium  and  magnesium 
(as  sulphates)  and  of  silica,  and  iron  and  aluminum  oxides  (as 
such)  ;  the  remainder  is  considered  to  be  sodium  sulphate  and  is 
multiplied  by  .3238  to  convert  it  to  sodium  (Na). 

5.     SILICA 

Moisten  the  residue  from  "4"  with  concentrated  hydrochloric- 
acid  and  evaporate  to  dryness  on  a  water  bath.  Moisten  again 
with  concentrated  hydrochloric  acid,  cover  the  dish,  and  digest 
for  5 — 10  minutes  on  the  bath.  Add  sufficient  water  to  dissolve  the 
salts  and  heat  again  on  the  bath  until  solution  is  complete.  Filter, 
wash  with  hot  water,  dry,  ignite,  and  weigh  the  silica  (Si02). 


*The  amount  should  be  sufficient  to  give,  if  possible,  0.5  gram  of 
total  solids  and  in  any  case  not  less  than  0.2  gram.  A  preliminary 
determination  made  by  evaporating  50  ml  of  the  water  will  show  the 
amount  required. 

fThe  "radiator"  recommended  by  Hillebrand  is  especially  good  for 
volatilizing  sulphuric  acid.  See  Chap.  XXIII,  15. 


XVII.      WATER  143 

6.    IRON 

To  the  filtrate  from  "5"  add  several  milliliters  of  bromine 
water,  or  a  few  drops  of  concentrated  nitric  acid,  and  boil.  Then 
cool  somewhat,  add  enough  hydrochloric  acid  to  insure  a  total  of 
10 — 15  ml  of  strong  acid,  make  slightly  alkaline  with  ammonium 
hydroxide,  and  boil  for  a  few  moments.  The  ammonia  should  not 
lie  iu  such  excess  as  to  require  long  boiling  to  expel  the  most  of  it, 
nor  is  the  expulsion  of  the  whole  of  it  necessary  or  desirable. 
Filter  as  soon  as  the  precipitate  settles,  wash  with  hot  water,  ignite, 
and  weigh  as  Fe203  +  A1203.  Report  the  iron  and  aluminum 
together  as  iron.  Multiply  the  weight  of  the  precipitate  by  .6994 
to  obtain  the  iron  (Fe)  equivalent. 

7.     CALCIUM 

Heat  the  filtrate  from  "  6  "  to  boiling,  and  to  the  boiling  solu- 
tion add  gradually  about  10  ml  of  ammonium  oxalate  solution. 
Filter  after  standing  for  at  least  one  hour,  wash  two  or  three  times 
with  hot  water,  and  determine  gravimetrically  as  oxide  or  sulphate 
as  described  under  "Limestone,"  Chap.  XVI,  5.  Multiply  the 
weight  of  CaO  by  .7146,  or  of  CaS04  by  .2944  to  convert  to 
calcium  (Ca). 

8.     MAGNESIUM 

To  the  filtrate  from  "7"  add  10  ml  of  sodium  ammonium 
phosphate  or  disodium  hydrogen  phosphate  solution.  After  vig- 
orous stirring  add  ammonium  hydroxide  in  considerable  excess. 
After  standing  over  night,  filter,  and  wash  with  dilute  ammonium 
hydroxide  (ammonium  hydroxide  of  0.90  sp.  gr.  diluted  to  10 
times  its  volume).  Char  the  paper  slowly  without  allowing  it  to 
ignite,  burn  off  the  carbon  over  a  gradually  increasing  flame,  then 
apply  a  weak  blast  for  a  long  time  and  repeat  to  constant  weight. 
\V»'i«:h  as  Mg.,P.,0-  and  multiply  by  .2184  to  convert  to  magne- 
sium (Mg). 

9.     CHLORINE 
REAGENTS 

(a)  Sulphuric  acid  of  about  N/28  strength:     This  solution 
does  not  have  to  be  standardized. 

(b)  Sodium  carbonate  solution  of  about  N/28  strength:  This 
solution  does  not  have  to  be  standardized. 


144  METHODS  OF  ANALYSIS 

(c)  Potassium   chromate    indicator:     Dissolve    5    grams    of 
potassium  chromate  in  water,  add  a  solution  of  silver  nitrate  drop 
by  drop  until  a  slight  permanent  red  precipitate  is  produced,  filter, 
and  dilute  to  100  ml. 

(d)  Standard  sodium  chloride  solution:     Several  grams  of 
C.  P.  sodium  chloride  are  finely  powdered  and  heated  for  five 
minutes,  not  quite  to  redness.    When  cold,  0.8243  gram  is  dissolved 
in  water  and  made  up  to  500  ml.    Each  ml  =  0.001  gram  chlorine. 

(e)  Standard  silver  nitrate  solution:    Dissolve  about  5  grams 
of  C.  P.  silver  nitrate  in  water  and  dilute  to  1  liter. 

STANDARDIZATION 

Transfer  25  ml  of  the  standard  sodium  chloride  solution  to 
a  porcelain  dish,  or  a  beaker  standing  on  a  white  surface.  Dilute 
with  75  ml  of  chlorine-free  water.  Add  1  ml  of  the  potassium 
chromate,  and  introduce  the  silver  nitrate  from  a  burette  until  a 
faint  red  color  of  silver  chromate  remains  permanent  on  stirring. 
Correct  for  the  amount  of  silver  nitrate  necessary  to  give  in  100 
ml  of  chlorine-free  water,  with  1  ml  of  the  chromate,  the  shade 
obtained  at  the  end  of  the  titration  of  the  sodium  chloride  solution. 
From  2  or  3  of  such  titrations  calculate  the  strength  of  the  silver 
nitrate  Solution. 

DETERMINATION 

To  100  ml  of  the  water  add  a  few  drops  of  phenolphthalein. 
If  a  red  color  appears,  titrate  the  carbonates  thus  indicated  to 
bicarbonates  with  the  sulphuric  acid  solution  (a).  If  the  water  is 
acid  to  methyl  orange,  add  the  sodium  carbonate  solution  (b), 
from  a  burette  until  the  acidity  is  neutralized.  Add  1  ml  of  the 
chromate  and  titrate  with  the  standard  silver  nitrate.  Correct 
for  the  amount  of  silver  nitrate  necessary  to  give  in  100  ml  of 
chlorine-free  water,  with  1  ml  of  the  chromate,  the  shade  obtained 
at  the  end  of  the  titration  of  the  sample. 

NOTE:  Greater  accuracy  is  secured  by  operating  in  yellow 
light.  Gas  or  electric  light  is  better  than  daylight. 

10.     SULPHURIC  ACID 

Acidify  300  ml,  or  a  suitable  amount,  of  the  water  slightly 
with  hydrochloric  acid.  Heat  to  boiling  and  add  drop  by  drop 
5 — 10  ml  of  a  hot,  10  per  cent  barium  chloride  solution.  After 
standing  over  night,  filter,  wash  free  from  chlorine  with  hot  water, 


XVII.      WATER  145 

ignite,  and  weigh  as  barium  sulphate  (BaSOJ.  Add  a  drop  of 
sulphuric  and  hydrofluoric  acids  before  finishing  the  ignition;  this 
will  remove  any  silica,  if  present,  and  convert  any  reduced  barium 
sulphide  back  to  sulphate.  Multiply  by  .4115  to  convert  to  S04. 

11.     CARBONIC  ACID 

Carbonic  acid  (CO3)  is  determined  by  difference,  as  the 
amount  necessary  to  saturate  the  excess  of  basic  over  acid  ions. 

12.  ORGANIC  AND  VOLATILE  MATTER. 

This  is  taken  as  the  difference  between  the  "total  solids"  and 
the  sum  of  the  other  constituents  determined. 

13.     SUSPENDED  MATTER 

This  determination  need  not  be  made  except  in  the  case  of  raw 
waters  for  new  factory  sites  or  of  other  waters  where  the  amount 
is  visibly  excessive.  Determine  by  making  a  total  solids  determina- 
tion on  the  unfiltered  water,  being  careful  that  the  sample  is  well 
mixed  so  that  the  portion  taken  will  contain  its  proper  proportion 
of  insoluble  matter.  The  difference  between  the  total  solids  deter- 
mined in  this  manner  and  determined  as  in  "3"  represents  the 
amount  of  "suspended  matter."  Record  the  "suspended  matter" 
as  a  separate  figure  and  do  not  include  in  the  "total  solids"  in 
the  statement  of  the  analysis. 

14.  HYPOTHETICAL  COMBINATIONS 
R-eport  the  basic  and  acid  ions  and  the  hypothetical  combina- 
tions in  terms  of  parts  per  100,000.  In  calculating  the  hypothetical 
combinations  join  the  basic  ions  in  the  following  order :  potassium, 
sodium,  magnesium,  calcium,  and  iron,  to  the  acid  ions  in  the 
following  order:  chlorine,  sulphuric  acid,  and  carbonic  acid. 
Report  silica  as  free  SiO2. 

15.     EXAMPLE 
An  analysis  showed  the  following  (parts  per  100,000)  : 

Total   Solids   45.22 

Total  Sulphates 50.26 

SiO,    3.80 

Fe263  and  A12O3 20  (X  .6994  =       .14  Fe) 

CaO    5.12  ( X  -7146  =  =    3.66  Ca) 

Mg2P207   6.7T  (X  .2184  =    1.48  Mg) 

Cl    2.17 

BaS04  29.74  ( X  .4115  =  12.24  S0<)      ' 


146 


METHODS  OF  ANALYSIS 


CALCULATION  OF  SODIUM 


5.12  CaO  X  2.4279 
6.77  MgaP2O7X  1.0810 
50.26—  (3.80  +  .20  +  12.43 
26.51  Na^SO,  X  .3238 


7.32) 


—  12.43  CaSO4 
=    7.32  MgS04 
=  26.51  Na2SO4 
=    8.58  Na 


CALCULATION  OF  SALTS  AND  CARBONIC  ACID 


2.17  Cl  X  .6486 

2.17  Cl  +  1.41  Na 

8.58  Na  — 1.41  Na 

12.24  SO4  X  .4789 

12.24  SO4  +  5.86  Na 

7.17  Na  — 5.86  Na 

1.31  Na  X  2.3045 

1.48  Mg  X  3.4673 

3.66  Ca  X  2.4975 

.14  Fe  X  2.0746 

(3.02  +  5.13  +  9.14  -f  .29)  —  (1.31 


=    1.41  Na 

—  3.58  NaCI 

=r    7.17  Na   (uncombined) 
=    5.86  Na 

—  18.10  Na2SO4 

=    1.31  Na  (uncombined) 
=    3.02  Na,CO3 
r=    5.13  MgCO3 
=    9.14  CaCO3 
=      .29  FeCO, 
1.48  +  3.66  +  .14)    —  10.99  CO3 


16.     STATEMENT  OF  ANALYSIS 
The  above  analysis  will  then  be  stated  as  follows: 


Silica SiO2 

Iron Fe 

Calcium Ca 

Magnesium Mg 

Sodium .Na 

Chlorine .Cl 

Sulphuric  Acid SO4 

Carbonic  Acid CO3 


Parts  per 

100,000 
3.80 
.14 
3.66 
1.48 
8.58 
2.17 
12.24 
10.99 


Hypothetical 
Combinations 


43.06 

Organic  and  Volatile  Matter 
(by  difference) 2.16 

Total  Solids..  ..45.22 


Parts  per 
100,000 


Silica SKV 

Sodium  Chloride NaCI 

Sodium  Sulphate Na2SO4 

Sodium  Carbonate Na2CO3 

Magnesium   Carbonate.  .  .MgCO3 

Calcium   Carbonate .CaCO3 

Ferrous  Carbonate FeCO3 


3.80 
3.58 
18.101 
3.02) 
5.13 
9.141 
.29 

43.06 
Organic  and  Volatile  Matter 

(by  difference) ! 2.16 

Total    Solids    .  ..45.22- 


XVIII.     DIATOMACEOUS  EARTH  (KIESELGUHR) 

For  judging-  the  suitability  of  diatomaceous  earth  for  filtra- 
tion work,  no  chemical  analysis  will  probably  be  of  as  much  value 
as  an  actual  fitration  test,  but  in  most  cases  the  apparent  specific 
gravity  will  furnish  a  good  index.  The  lower  the  apparent  specific 
gravity,  the  better  is  the  quality  of  the  material.  The  silica  deter- 
mination will  give  only  a  general  idea  of  the  purity. 

1.     SAMPLING 

Take  an  average  sample  of  each  lot  received,  mix  well,  and 
preserve  a  suitable  amount  in  a  stoppered  bottle. 

2.    APPARENT  SPECIFIC  GRAVITY  (POUNDS  PER 
CUBIC  FOOT) 

The  weight  per  cubic  foot  is  taken  as  the  weight  of  the  mate- 
rial which  occupies  one  cubic  foot  of  space  under  the  conditions 
specified,  without  packing,  and  is  obtained  as  follows : 

Shake  the  material  through  a  20  mesh  sieve  held  1  inch  above 
the  top  of  a  25  ml  porcelain  crucible  of  known  weight  and  capacity, 
returning  to  the  sieve  the  portion  which  falls  outside  the  crucible, 
until  the  crucible  is  completely  filled.  Then  level  off  with  a 
spatula,  avoiding  any  packing,  and  weigh  to  the  nearest  centigram. 
Make  this  determination  in  triplicate. 

If  W  =  weight  in  grams  of  the  material  in  the  crucible, 
V  ==  volume  of  the  crucible  in  milliliters,  and  X  ==  apparent  spe- 
cific gravity  of  the  material  in  "pounds  per  cubic  foot,"  then 

_,        62.43  W 
~^~ 

Or,  if  the  crucible  holds  exactly  25  ml,  tlu-n 

x     10  w 

4 


148  METHODS  OF  ANALYSIS 

3.    MOISTURE 

Heat  0.5  gram  for  3  hours  in  a  porcelain  crucible  in  a  drying 
oven  at  100 — 105°,  and  then  for  successive  periods  of  one  hour 
until  the  weight  is  constant.  Report  the  loss  in  weight  as  moisture. 

4.  ORGANIC  AND  VOLATILE  MATTER 

Heat  the  crucible  containing  the  dried  sample  from  "3"  to 
full  redness  over  a  good  burner  or  in,  an  electric  furnace,  and 
ignite  to  constant  weight.  The  loss  in  weight  of  the  dried  sample 
represents  the  amount  of  "organic  and  volatile  matter." 

5.     SILICA 

Mix  0.5  gram  of  the  material  thoroughly  with  4 — 6  parts  of 
sodium  carbonate  in  a  platinum  crucible,  and  fuse.  When  the 
fusion  is  complete,  allow  to  cool,  and  extract  the  melt  with  water 
and  hydrochloric  acid.  Evaporate  to  dryness  on  the  water  bath, 
and  proceed  as  in  Chap.  XIII,  2,  repeating  the  evaporation  and 
nitration  until  all  the  silica  is  removed.  Ignite  the  residue  to 
constant  weight,  using  a  blast  lamp  or  electric  furnace  for  the 
final  ignition,  and  weigh  as  Si02. 


XIX.     SULPHUR 

1.     SAMPLING  AND   PREPARATION   OF   SAMPLE 

A  laboratory  employe  should  sample  each  car  of  sulphur  re- 
ceived, by  taking  representative  samples  from  different  parts  of 
the  car.  Crush  the  entire  sample  to  V±  inch  size  with  a  jaw 
crusher.  Mix  the  crushed  sample,  and  reduce  it  by  quartering. 
Grind  to  60  mesh  size  in  a  mortar  or  on  a  bucking  board,  and 
preserve  a  suitable  amount  in  a  stoppered  bottle.  A  disc  pulver- 
izer is  not  suitable,  because  the  friction  heats  the  sulphur  and 
causes  it  to  become  viscous. 


2.     MOISTURE 

Heat  1  gram  for  exactly  one  hour  in  a  porcelain  crucible  in 
a  drying  oven  at  100 — 105°.    Report  the  loss  in  weight  as  moisture. 


3.    ASH 

Heat  the  crucible  containing  the  dried  sample  from  "2"  until 
the  sulphur  ignites,  then  remove  the  flame  and  allow  the  sulphur 
to  burn.  When  combustion  has  ceased,  heat  to  full  redness  to 
constant  weight,  cool,  and  weigh  the  residue. 

4.    SULPHUR 

(a)  Method  I:  Weigh  out  about  0.1  gram  and  transfer  to 
a  flask  of  250  ml  capacity.  Add  25  ml  of  a  strong  potassium 
hydroxide  solution,  and  heat  in  a  water  bath  until  the  sulphur 
is  all  dissolved  (about  one-half  hour  is  required).  Cool,  add 
200  ml  of  freshly  prepared  bromine  water  and  heat  until  the 
sulphur  is  all  oxidized,  adding  more  bromine  water  if  necessary. 
Transfer  to  a  beaker,  make  slightly  acid  with  hydrochloric  acid 
and  boil  until  the  excess  of  bromine  is  expelled,  then  filter  and 


150  METHODS  OF  ANALYSIS 

wash  with  hot  water.    Precipitate  the  sulphuric  acid  in  the  filtrate 
with  barium  chloride,  following  the  procedure  in  Chap.  XIII,  8. 

(b)  *Method  II:  Dissolve  about  0.1  gram  in  1  ml  of  dry 
liquid  bromine  and,  add  10  ml  of  concentrated  nitric  acid.  Re- 
move the  excess  of  bromine  and  the  nitrous  fumes  by  heat,  add 
100  ml  of  water  and  several  ml  of  hydrochloric  acid,  and  boil  to 
expel  the  rest  of  the  nitric  acid.  Then  precipitate  the  sulphuric 
acid  with  barjum  chloride  in  the  regular  manner. 

5.     ARSENIC 

Test  qualitatively  for  arsenic  as  follows :  Shake  approxi- 
mately 1  gram  of  the  ground  sample  with  15  drops  of  strong 
ammonium  hydroxide  and  2  ml  of  water.  Filter  after  half  an 
hour,  and  to  the  clear  filtrate  in  a  test  tube  add  30  drops  of  con- 
centrated hydrochloric  acid  and  15  drops  of  a  10  per  cent  solution 
of  oxalic  acid.  Place  a  strip  of  bright  copper  foil  in  the  solution 
and  heat  to  60 — 100° ;  in  the  presence  of  arsenic  an  iron-colored  to 
black  film  forms  immediately  on  the  copper.  If  the  presence  of 
arsenic  is  indicated,  always  check  the  reagents  by  a  blank  test. 


*Bjerregaard,  Jour.  Ind.  and  Eng.  Chem.,  11,  1055. 


XX.     FOODS  AND  FEEDING  STUFFS 

The  methods  are  in  general  those  of  the  Association  of  Official 
Agricultural  Chemists. 

1.     PREPARATION  OP  SAMPLE 

Grind  the  sample  so  that  it  will  pass  through  a  sieve  having 
circular  openings  1/25  inch  (1  mm)  in  diameter.  If  the  sample 
cannot  be  ground,  reduce  it  to  as  fine  a  state  as  possible.  Deter- 
mine moisture  in  both  the  original  and  the  ground  sample,  and 
correct  the  results  of  the  analysis  for  any  change  in  the  moisture 
content  during  grinding. 

2.     MOISTURE 

Weigh  out  10  grams  in  a  3  x  %  inch  aluminum  dish,  provided 
with  a  cover,  and  dry  in  vacuo  at  100 — 105°  for  3 — 4  hours,  and 
then  for  successive  periods  of  one  hour  until  the  loss  of  weight  in 
one  hour  is  not  over  0.1%. 

3.     CRUDE  PROTEIN 

Determine  nitrogen  by  one  of  the  following  methods,  and 
multiply  the  result  by  6.25  to  convert  to  protein. 

KJELDAHL  METHOD 
REAGENTS 

For  ordinary  work  N/2  acid  is  recommended.  For  work  in 
determining  very  small  amounts  of  nitrogen  N/10  acid  is  recom- 
mended. In  titrating  mineral  acids  against  ammonium  hydroxide 
solution  use  cochineal  or  methyl  red  as  indicator. 

(a)  Standard  sulphuric  acid:  Determine  the  absolute 
strength  of  the  acid  by  precipitation  with  barium  chloride  solution 
as  follows :  Dilute  a  measured  quantiy  of  the  acid  to  be  stand- 
ardized to  approximately  100  ml,  heat  to  boiling  and  add  drop  by 


152  METHODS  OF  ANALYSIS 

drop  a  10%  solution  of  barium  chloride  until  no  further  precipi- 
tation occurs.  Continue  the  boiling  for  about  5  minutes,  allow 
to  stand  for  5  hours  or  longer  in  a  warm  place,  pour  the  super- 
natant liquid  on  a  tared  Gooch  or  on  an  ashless  filter,  treat  the 
precipitate  with  25 — 30  ml  of  boiling  water,  transfer  to  the  filter 
and  wash  with  boiling  water  until  the  filtrate  is  free  from  chlorine. 
Dry,  ignite  over  a  Bunsen  burner  and  weigh  as  barium  sulphate. 
See  also  Chap.  XXV,  21  (a)  (3).  A  normal  solution  of  sulphuric 
acid  has  the  following  equivalents : 

1  ml  =  .04904  gram  H2S04 
1  ml  =  .01401  gram  N 
1  ml  =  .01703  gram  NH3 

(b)  Standard    alkali    solution:      Accurately    determine    the 
strength  of  this  solution  by  titration  against  the  standard  acid. 
N/10  solution  is  recommended. 

(c)  Sulphuric  acid:     Of  sp.  gr.  1.84  and  free  from  nitrates 
and  ammonium  sulphate. 

(d)  Metallic  mercury,   or  mercuric   oxide:    Mercuric  oxide 
should  be  prepared  in  the  wet  way,  but  not  from  mercuric  nitrate. 

(e)  Copper  sulphate:     Crystallized. 

(f)  Potassium  permanganate:     Finely  pulverized. 

(g)  Granulated  zinc  or  pumice  stone:     Added  to  the  con- 
tents of  the  distillation  flask  if  necessary  to  prevent  bumping. 

(h)  Potassium  sulphide  solution:  Dissolve  40  grams  of 
commercial  potassium  sulphide  in  1  liter  of  water. 

(i)  Sodium  hydroxide  solution:  A  saturated  solution,  free 
from  nitrates. 

(j)  Cochineal  solution:  Digest,  with  frequent  agitation,  3 
grams  of  pulverized  cochineal  in  a  mixture  of  50  ml  of  strong 
alcohol  and  200  ml  of  water  for  1  or  2  days  at  ordinary  tempera- 
ture, and  then  filter. 

(k)     Methyl  red  solution:     Dissolve  1  gram  of  methyl  red 
(dimethyl-amino-azo-benzene  ortho-carbonic    acid)    in    100   ml    of 
95%  alcohol. 
APPARATUS 

(a)  Kjeldahl  flasks  for  both  digestion  and  distillation: 
Total  capacity  of  about  550  ml,  made  of  hard,  moderately  thick, 
and  well-annealed  glass. 


XX.      POODS  AND  FEEDING  STUFFS  153 

(b)  Distillation  flasks:  For  distillation  any  suitable  flask 
of  about  550  ml  capacity  may  be  used.  It  is  fitted  with  a  rubber 
stopper  through  which  passes  the  lower  end  of  a  Kjeldahl  con- 
noting bulb  to  prevent  sodium  hydroxide  being  carried  over 
mechanically  during  distillation.  The  bulb  should  be  about  3  cm 
in  diameter,  and  the  tubes  should  be  of  the  same  diameter  as  the 
condenser  tube  with  which  the  upper  end  of  the  bulb  tube  is  con- 
nected by  means  of  rubber  tubing. 

DETERMINATION 

Place  0.7 — 3.5  grams,  according  to  the  nitrogen  content,  of  the 
substance  to  be  analyzed  in  a  digestion  flask  with  approximately 
0.7  gram  of  mercuric  oxide,  or  its  equivalent  in  metallic  mercury, 
and  add  20 — 30  ml  of  sulphuric  acid  0.1 — 0.3  gram  of  crystallized 
copper  sulphate  may  also  be  used  in  addition  to  the  mercury,  or 
in  place  of  it).  Place  the  flask  in  an  inclined  position  and  heat 
below  the  boiling  point  of  the  acid  until  frothing  has  ceased.  (A 
small  piece  of  paraffin  may  be  added  to  prevent  excessive  foaming. ) 
Then  raise  the  heat  until  the  acid  boils  briskly  and  digest  for  a 
time  after  the  mixture  is  colorless  or  nearly  so,  or  until  oxidation 
is  complete.  Remove  the  flask  from  the  flame,  hold  it  upright,  and 
while  still  hot  add  carefully  potassium  permanganate  in  small 
quantities  at  a  time  until,  after  shaking,  the  liquid  remains  green 
or  purple. 

After  cooling  dilute  with  about  200  ml  of  water,  add  a  few 
pieces  of  granulated  zinc  or  pumice  stone,  if  necessary  to  prevent 
bumping,  and  25  ml  of  potassium  sulphide  solution  with  shaking. 
Next  add  sufficient  sodium  hydroxide  solution  to  make  the  reaction 
strongly  alkaline  (50  ml  is  usually  enough)  pouring  it  down  the 
side  of  the  flask  so  that  it  does  not  mix  at  once  with  the  acid  solu- 
tion. Connect  the  flask  immediately  with  the  condenser,  mix  the 
contents  by  shaking,  distil  into  a  measured  quantity  of  the  standard 
acid  until  all  ammonia  has  passed  over,  and  titrate  with  the  stand- 
ard alkali.  The  first  150  ml  of  the  distillate  will  generally  contain 
all  the  ammonia. 

The  use  of  mercuric  oxide  in  this  operation  greatly  shortens 
the  time  necessary  for  digestion,  which  is  rarely  over  an  hour  and 
a  half  in  case  of  substances  most  difficult  to  oxidize,  and  is  more 
'•ommonly  less  than  an  hour.  In  most  instances  the  use  of  potas- 
Hum  permanganate  is  quite  unnecessary,  but  it  is  believed  that  in 
•  xreptiomil  cases  it  is  required  for  complete  oxidation,  and  in 
view  of  the  uncertainty  it  is  always  used.  The  potassium  sulphide 


154  METHODS  OF  ANALYSIS 

removes  all  the  mercury  from  the  solution,  and  so  prevents  the 
formation  of  mercuro-ammoiiium  compounds  which  are  not  com- 
pletely decomposed  by  the  sodium  hydroxide.  The  addition  of 
zinc  gives  rise  to  an  evolution  of  hydrogen  and  prevents  violent 
bumping. 

Previous  to  use  the  reagents  should  be  tested  by  a  blank 
experiment  with  sugar.  The  sugar  partially  reduces  any  nitrates 
present  that  might  otherwise  escape  notice. 

GUNNING  METHOD 
REAGENTS 

Potassium  sulphate:    Pulverized. 

The  other  reagents  and  standard  solutions  used  are  described 
above. 

APPARATUS 

The  apparatus  used  is  described  above. 

DETERMINATION 

Place  0.7 — 3.5  grams,  according  to  the  nitrogen  content,  of 
the  substance  to  be  analyzed  in  a  digestion  flask.  Add  10  grams 
of  powdered  potassium  sulphate  and  15 — 25  ml  (ordinarily  about 
20  ml)  of  sulphuric  acid  (0.1 — 0.3  gram  of  crystallized  copper 
sulphate  may  also  be  added).  Conduct  the  digestion  as  in  the 
Kjeldahl  process,  starting  with  a  temperature  below  the  boiling 
point  and  increasing  the  heat  gradually  until  frothing  ceases. 
Digest  for  a  time  after  the  mixture  is  colorless  or  nearly  so,  or 
until  oxidation  is  complete.  Do  not  add  either  potassium  per- 
manganate or  potassium  sulphide.  Cool,  dilute,  neutralize,  distil, 
and  titrate  with  the  standard  alkali.  In  neutralizing  before  distil- 
ling it  is  convenient  to  add  a  few  drops  of  phenolphthalein  indi- 
cator or  litmus  paper.  The  pink  color  given  by  phenolphthalein 
indicating  an  alkaline  reaction  is  destroyed  by  a  considerable 
excess  of  strong  fixed  alkali. 

KjELDAHL-GuNNiNG- ARNOLD   METHOD 

REAGENTS  AND  APPARATUS 
Described  above. 

DETERMINATION 

Place  0.7 — 3.5  grams,  according  to  the  nitrogen  content,  of  the 
substance  to  be  analyzed  in  a  digestion  flask.  Add  15 — 18  grams 
of  potassium  sulphate,  1  gram  of  copper  sulphate,  1  gram  of 
mercuric  oxide,  or  its  equivalent  in  metallic  mercury,  and  25  ml 
of  sulphuric  acid.  Heat  gently  until  frothing  ceases,  then  boil 
the  mixture  briskly,  and  continue  the  digestion  for  a  time  after 


XX.      FOODS  AND  FEEDING  STUFFS  155 

the  mixture  is  colorless  or  nearly  so  or  until  oxidation  is  complete. 
Cool,  dilute  with  about  200  ml  of  water,  add  50  ml  of  potassium 
sulphide  solution,  make  strongly  alkaline  with  sodium  hydroxide 
solution  and  complete  the  determination  as  directed  in  the  Kjel- 
<  la  111  method. 

4.     CRUDE  FAT 

REAGENTS 

(a)  Anhydrous  Ether:  Use  particular  care  in  the  purifi- 
cation of  the  ether.  Wash  ethyl  ether,  containing  not  more  than 
4' ,  alcohol,  with  4  or  5  successive  portions  of  distilled  water,  add 
solid  sodium  or  potassium  hydroxide,  and  let  stand  until  most  of 
the  water  has  been  abstracted  from  the  ether.  Decant  into  a  dry 
bottle  and  add  small  pieces  of  carefully  cleaned  metallic  sodium. 
It  will  be  found  that  a  considerable  quantity  of  sodium  is  needed 
to  remove,  the  last  traces  of  water  although  little  of  the  sodium 
appears  to  be  used  up  in  the  process ;  the  sodium  should  therefore 
be  added  on  each  of  several  different  days  until  no  more  hydrogen 
is  liberated  from  the  fresh  pieces.  Keep  the  ether,  thus  dehy- 
drated, over  metallic  sodium  in  lightly  stoppered  bottles.  Use 
glass  stoppered,  and  not  cork  stoppered  bottles.  If  a  brown  pre- 
cipitate develops,  which  indicates  that  the  washing  was  incom- 
plete, repurify  the  ether.  Test  each  lot  of  ether  for  insoluble  resi- 
due by  evaporating  a  measured  volume. 

APPARAT 

Use  an  extraction  apparatus  attached  to  the  flask  by  a  ground 
id  ass  joint  cr  a  mercury  seal,  and  not  by  a  cork  or  rubber  stopper. 
Alunduni  extraction  shells  are  recommended. 

DETERMINATION 

Large  quantities  of  soluble  carbohydrates  may  interfere  with 
the  complete  extraction  of  the  fat.  In  such  cases  extract  with 
\vater  before  proceeding  with  the  determination. 

Dry  about  2  grams  of  the  material  thoroughly  in  a  drying 
oven  at  100 — 105°.  Extract  with  the  anhydrous  ether  for  16  hours. 
Filter  the  extract  through  filter  paper  to  remove  solid  particles, 
usinjr  ether  for  washing.  Evaporate  the  extract  and  washings 
carefully  to  drynoss,  and  dry  at  100 — 105°  for  30  minutes,  cool 
in  a  desiccator,  a.ul  weigh.  Continue  the  drying  by  half-hour 
periods  until  a  minimum  weight  is  obtained.  For  most  feeds  a 
period  of  1  to  11/^  hours  is  required.  Save  the  residue  for  the 
crude  fiber  determination. 


156  METHODS  OF  ANALYSIS 

5.     CRUDE  FIBER 

REAGENTS 

(a)  1.25%   Sulphuric  Acid  Solution:     Exact  strength,   de- 
termined by  titration. 

(b)  1.25%    Sodium   Hydroxide   Solution:     Exact   strength, 
determined  by  titration. 

DETERMINATION 

Extract  a  quantity  of  the  substance,  representing  about  2 
grams  of  the  dry  material,  with  ordinary  ether,  or  use  the  residue 
from  the  determination  of  the  ether  extract.  To  this  residue  in 
a  500  ml  flask  add  200  ml  of  boiling  1.25%  sulphuric  acid;  connect 
the  flask  with  an  inverted  condenser,  the  tube  of  which  passes  only 
a  short  distance  beyond  the  rubber  stopper  into  the  flask,  or  simply 
cover  a  tall  conical  flask,  which  is  well  suited  for  this  determina- 
tion, with  a  watch  glass  or  short  stemmed  funnel,  boil  at  once  and 
continue  boiling  gently  for  30  minutes.  A  blast  of  air  conducted 
into  the  flask  will  serve  to  reduce  the  frothing  of  the  liquid.  Filter 
through  linen  and  wash  with  boiling  water  until  the  washings  are 
no  longer  acid ;  rinse  the  substance  back  into  the  flask  with  200 
ml  of  boiling,  1.25%  solution  of  sodium  hydroxide,  free  or  nearly 
free  from  sodium  carbonate,  boil  at  once,  and  continue  boiling 
gently  for  30  minutes  as  directed  above  for  the  treatment  with 
acid,  filter  at  once  rapidly,  and  wash  with  boiling  water  until  the 
washings  are  neutral.  The  last  filtration  may  be  performed  upon 
a  Grooch  crucible,  a  linen  filter,  or  a  tared  filter  paper.  If  a  linen 
filter  is  used,  rinse  the  crude  fiber,  after  washing  is  completed,  into 
a  flat-bottom  platinum  dish  by  means  of  a  jet  of  water;  evapo- 
rate to  dryness  on  a  steam  bath,  dry  to  constant  weight  at  110°  C., 
weigh,  incinerate  completely,  and  weigh  again.  The  loss  in  weight 
is  considered  to  be  crude  fiber.  If  a  tared  filter  paper  is  used, 
weigh  in  a  weighing  bottle.  In  any  case  the  crude  fiber  after 
drying  to  constant  weight  at  110°  C.  must  be  incinerated  and  the 
amount  of  the  ash  deducted  from  the  original  weight. 

6.     ASH 

Weigh  out  about  2  grams  and  determine  ash  by  the  lixiviation 
method  as  described  in  Chap.  I,  7  (b). 

7.     NITROGEN-FREE   EXTRACT 

Subtract  from  100  the  sum  of  the  percentages  of  moisture, 
crude  protein,  crude  fat,  crude  fiber,  and  ash. 


XXI.     COTTON  SEED  CAKE 

Sample  tach  car  of  cotton  seed  cake  received,  and  determine 
moisture  and  protein. 

1.     SAMPLING 

Take  a  *handful  of  cake  from  each  of  at  least  25  bags  selected 
promiscuously  throughout  the  car,  the  total  sample  amounting  to 
at  least  10  pounds.  If  possible,  sample  a  greater  number  of  bags. 
Mix  the  sample,  remove  a  quart  with  a  scoop,  and  preserve  in  a 
suitable  container  as  a  reference  sample  for  size  only,  and  so 
labeled. 

2.     PREPARATION  OF  SAMPLES 

If  the  original  sample  exceeds  15 — 20  pounds,  reduce  to  this 
amount,  but  not  below,  by  halving  or  quartering;  otherwise  grind 
the  entire  remainder  of  the  original  sample  on  a  bucking  board, 
or  by  means  of  other  suitable  apparatus,  to  such  an  extent  that 
the  largest  lumps  will  not  exceed  VL  inch  in  size,  mix  thoroughly, 
and  quarter  once.  Repeat  the  procedure  of  grinding  and  quar- 
tering until  about  3  pints  of  material  remain.  Mix  thoroughly 
nnd  make  up  3  samples  of  about  1  pint  each,  using  fruit  jars  or 
other  suitable,  tightly  sealed  containers.  Label  each  sample  with 
the  car  number,  date  of  receipt  and  the  name  of  the  factory  where 
received. 

Retain  two  of  the  above  samples  as  referee  samples  for 
analysis,  subject  to  shipping  instructions  from  the  General  Office. 
Use  a  third  sample  for  the  laboratory  analysis,  and  seal  and  save 
for  future  reference  the  portion  of  this  sample  left  over  from  the 
analysis. 

Prepare  the  sample  for  analysis  by  putting  the  entire  sample 
through  a  sieve  having  circular  openings  1  mm  in  diameter,  grind- 


*The  directions  refer  to  "screened  cracked  cake." 


158  METHODS  OF  ANALYSIS 

ing  the  portion  retained  by  the  sieve  until  all  the  particles  pass 
through,  then  mix  the  sample  thoroughly  to  destroy  the  segregation 
of  the  hulls,  which  are  more  difficult  to  reduce  to  the  necessary 
degree  of  fineness,  from  the  other  portion  of  the  sample.  To  avoid 
change  in  moisture  content,  grind  the  material  as  rapidly  as 
possible  and  do  not  allow  it  to  stand  exposed  to  the  air  unneces- 
sarily. 

3.  ANALYSIS 

Determine  moisture  and  protein  as  described  below.  The 
methods  are,  with  some  unimportant  modifications  in  wording, 
those  of  the  Interstate  Cotton  Seed  Crushers'  Association. 

4.  MOISTURE 

Heat  2  to  5  grams  for  3  hours  in  an  oven  at  a  temperature 
of  100°  C.,  using  an  aluminum  dish  2  inches  in  diameter,  provided 
with  a  cover.  As  soon  as  the  dish  is  removed  from  the  oven, 
cover  and  cool  in  a  desiccator.  Report  the  loss  in  weight  as 
moisture. 

5.     PROTEIN 

Digest  1.7512  grams  of  the  sample  with  approximately  0.5 
gram  of  metallic  mercury  or  0.7  gram  of  mercuric  oxide,  10  grams 
of  sodium  or  potassium  sulphate,  and  25  ml  of  sulphuric  acid 
(sp.  gr.  1.84).  Place  the  flask  in  an  inclined  position  and  heat  below 
the  boiling  point  of  the  acid  from  5  to  15  minutes,  or  until  frothing 
has  ceased.  Increase  the  temperature  and  continue  digestion  until 
the  liquid  becomes  colorless,  or  until  complete  digestion  is  obtained. 
The  process  is  the  same  from  now  on  as  in  the  regular  Kjeldahl 
method,  except  that  no  potassium  permanganate  is  added. 

Distillation:  After  cooling,  add  about  300  ml  of  distilled 
water,  a  few  pieces  of  zinc  to  keep  the  contents  of  the  flask  from 
bumping,  and  25  ml  of  a  4%  solution  of  potassium  or  sodium  sul- 
phide, or  a  sufficient  amount  to  precipitate  all  the  mercury.  After 
mixing  thoroughly,  add  60  ml  of  a  sodium  hydroxide  solution  of 
1.50  sp.  gr.,  or  sufficient  to  make  strongly  alkaline,  pouring  it  down 
the  side  of  the  flask  so  that  it  does  not  mix  at  once  with  the  acid 
solution.  Connect  the  flask  with  a  condenser  of  glass  or  block 
tin,  mix  the  contents  of  the  flask  by  shaking  and  distil  into  an 
accurately  measured  quantity  of  standard  sulphuric  acid  solution 


XXI.      COTTON  SEED  CAKE  159 

(N/2  recommended)  to  which  has  been  added  50  ml  of  distilled 
water,  until  at  least  200  ml  of  distillate  is  obtained,  taking  care 
that  the  delivery  tube  reaches  below  the  level  of  the  standard  acid. 
Then  titrate  the  distillate  with  standard  fixed  alkali  solution  (N/4 
sodium  hydroxide  recommended).  To  obtain  the  percentage  of 
protein,  multiply  the  number  of  milliliters  of  acid  neutralized  by 
the  distillate  by  2.5,  if  the  acid  is  of  exactly  N/2  strength.  The 
factor  for  the  conversion  of  nitrogen  to  protein  is  6.25. 

Precautions:  Be  sure  that  the  sample  for  analysis  has  been 
ground  to  pass  a  1  millimeter  sieve,  as  prescribed  in  "2."  Test 
the  reagents  by  a  blank  experiment  with  sugar,  and  make  any 
correction  found  necessary. 

Consult  Chap.  XX,  3,  for  fuller  details  regarding  the  protein 
determination. 


XXII,     SOIL 

The  methods  are  in  the  main  those  of  the  Association  of  Offi- 
cial Agricultural  Chemists,  which  should  be  consulted  for  full 
details.  Make  only  the  determinations  mentioned  below. 

If  possible  there  should  be  recorded  with  each  analysis  a 
history  of  the  soil,  covering  crop  rotation,  extent  of  manuring, 
the  depth  of  the  soil  if  less  than  12  inches,  and  the  nature  of  the 
subsoil. 


1.     SAMPLING  OF   SOIL 

Sampling  should  be  done  preferably  when  the  soil  is  rea- 
sonably dry.  Remove  from  the  surface  all  vegetable  material  not 
incorporated  with  the  soil,  and  take  out  an  amount  about  one 
square  foot  in  section  to  the  depth  of  the  plowed  soil;  if  virgin 
soil  is  sampled,  sample  to  a  depth  of  6  inches,  but  not  below  the 
level  of  the  subsoil.  Mix  on  an  oil  cloth ;  if  too  wet,  let  it  dry 
but  not  to  form  clods.  Do  this  in  different  parts  of  the  field,  and 
take  equal  amounts  of  the  individual  samples.  Mix  the  composite 
sample  thoroughly,  reduce  by  quartering  to  about  2 — 4  pounds, 
and  air-dry  in  a  cool,  well-ventilated  place. 

If  the  soil  is  less  than  6  inches  deep,  take  and  analyze  a 
separate  sample  of  the  subsoil. 

2.     PREPARATION  OF  SAMPLE 
Follow  the  method  of  the  A.  0.  A.  C. 

3.     MOISTURE,  VOLATILE  MATTER,  AND  TOTAL 
NITROGEN 

Follow  the  methods  of  the  A.  0.  A.  C.  The  moisture  found 
in  the  air-dry  soil  is  reported  as  "hygroscopic  moisture." 


XXII.      SOIL  161 

4.     MISCELLANEOUS  INORGANIC   CONSTITUENTS 

.Make  a  stiong  acid  digestion  of  the  soil  and  determine,  accord- 
ing to  tin-  A.  0.  A.  C.  methods: 

(a)  Insoluble  residue. 

(b)  Iron,  aluminum,  and  phosphoric  acid  (collectively). 

(c)  Manganese. 

(d)  Calcium. 

(e)  Phosphoric  acid. 

(f)  Sulphuric  acid. 

(g)  Potassium, 
(h)     Sodium. 

5.     CARBON   DIOXIDE 

Liberate  the  carbon  dioxide  with  acid  and  determine  by  the 
increase  in  weight  of  a  potash  bulb,  as  in  Chap.  XIV,  16. 

6.     HUMUS 

Place  10  grams  of  the  sample  in  a  Gooch  crucible,  extract  with 
\r/t  hydrochloric  acid  until  the  filtrate  gives  no  precipitate  with 
ammonium  hydroxide  and  ammonium  oxalate,  and  remove  the 
acid  by  washing  with  water.  Wash  the  contents  of  the  crucible 
(including  the  asbestos  filter)  into  a  glass  stoppered  cylinder, 
with  500  ml  of  49£  ammonium  hydroxide,  and  allow  to  remain, 
with  occasional  shaking,  for  24  hours.  During  this  time  the 
cylinder  is  inclined  as  much  as  possible  without  bringing  the 
contents  in  contact  with  the  stopper,  thus  allowing  the  soil  to 
settle  on  the  side  of  the  cylinder  and  exposing  a  very  large  surface 
to  the  action  of  the  ammonium  hydroxide.  Place  the  cylinder  in 
a  vertical  position  and  leave  for  12  hours,  to  allow  the  sediment 
to  settle.  Filter  the  supernatant  liquid  (the  filtrate  must  be 
perfectly  clear),  evaporate  an  aliquot,  dry  at  100°,  and  weigh. 
Then  ignite  the  residue  and  again  weigh.  Calculate  the  humus 
from  the  difference  in  weights  between  the  dried  and  ignited 
residues. 

7.     WATER  SOLUBLE 

Transfer  50  grams  of  the  air  dried  soil,  with  500  ml  of  water, 
to  a  1000  ml  tiask,  boil  for  half  an  hour,  and  let  stand  for  24 
hours  with  occasional  shaking.  Then  make  up  to  the  mark,  filter, 
evaporate  an  aliquot,  and  dry  at  100 — 105°  to  constant  weight. 


162  METHODS  OF  ANALYSIS 

8.     MECHANICAL  ANALYSIS 
(*T.'B.  Osborne's  Method) 

The  details  of  this  method  will  be  given  with  sufficient  minute- 
ness to  make  its  practice  possible  by  all  analysts. 

Selecting  the  Sample:  Several  pounds  of  air-dried,  fine  earth 
are  secured  by  passing  the  soil  through  a  sieve,  the  holes  of  which 
are  three  millimeters  in  diameter. 

Sifting:  Thirty  grams  of  the  above  fine  earth  are  stirred 
with  from  300  to  400  milliliters  of  water  and  then  thrown  suc- 
cessively; upon  sieves  with  circular  holes  of  1,  0.5,  and  0.25  milli- 
meter diameter  respectively.  By  means  of  successive  additions 
of  water  and  the  use  of  a  camel's  hair  brush,  all  the  fine  material 
is  made  to  pass  through  the  sieves  and  these  at  the  last  are  agi- 
tated under  water  in  a  shallow  dish  in  such  a  way  that  the  soil 
is  immersed.  The  finest  sieve  should  be  well  wet  with  water 
on  its  lower  surface  just  before  using.  The  finest  particles  which 
render  the  water  turbid  are  easily  washed  through.  The  turbid 
water  is  kept  separated  from  the  clear  water  which  comes  off 
with  the  last  portions  that  pass  the  sieves.  The  turbid  water 
usually  does  not  amount  to  more  than  one  liter. 

Elutriation:  The  elutriation  should  be  carried  on  so  as  to 
secure  three  grades  of  silt;  the  diameters  of  the  particles  ranging 
in  the  first  grades  from  0.25  to  0.05  millimeter,  in  the  second  grade 
from  0.05  to  0.01  millimeter,  and  in  the  third  grade  from  0.01 
millimeter  to  the  impalpable  powder.  The  term  sand  is  applied 
to  the  first  grade,  silt  to  the  second,  and  dust  or  dust  and  clay  to 
the  third.  After  the  turbid  liquid  from  the  sifting  has  stood  a 
short  time  it  is  decanted  from  the  sediment  and  after  standing 
until  a  slight  deposit  is  formed,  is  again  decanted  and  the  sedi- 
ment examined  with  a  microscope.  If  sand  is  present,  the  sub- 
sidence of  the  turbid  liquid  is  continued  until  no  more  sand  is 
deposited.  As  the  sand  subsides  rapidly  there  is  no  difficulty 
in  altogether  freeing  the  liquid  first  decanted  from  this  grade 
of  particles.  The  sediment  thus  obtained  contains  all  the  sand, 
a  part  of  the  dust  and  much  silt.  As  only  dust  and  the  finest 
silt  render  the  water  turbid  the  sediment  is  stirred  a  few  times 
with  a  fresh  quantity  of  water  and  decanted  after  standing  long 

*From  Wiley's  "Principles  and  Practice  of  Agricultural  Analysis,"  2d 
ed.,  Vol.  1,  p.  212. 


xxn.     SOIL  163 

enough  to  let  all  the  sand  settle.  When  the  water  decanted  is 
free  from  turbidity,  the  last  portions  of  the  soil  passing  through 
the  sieve  with  clear  water  are  added  to  the  sediment  arid  the 
decantations  continued  so  as  to  remove  most  of  the  silt.  When 
no  more  silt  can  be  easily  removed  from  the  sediment  without 
decanting  sand,  the  decantations  are  made  into  a  different  vessel 
and  the  subsidences  so  timed  as  to  remove  as  much  of  the  silt 
as  possible.  By  using  a  little  care,  at  least  three-quarters  of  the 
sand  are  thus  obtained  free  from  silt.  The  rest  of  the  sand  is 
mixed  with  the  greater  part  of  the  silt  which  has  been  decanted 
into  the  second  vessel.  The  size  of  the  smallest  particle  in  this 
vessel  is  determined  with  the  microscope,  to  make  sure  that  its 
contents  are  free  from  dust  as  they  usually  will  be  if,  after 
settling  for  a  few  moments,  they  leave  the  water  free  from 
turbidity. 

The  soil  is  thus  separated  into  three  portions,  one -containing 
sand,  one  sand  and  silt,  and  the  other  silt,  dust,  and  clay.  The 
sand  and  silt  are  separated  from  each  other  by  repeating  the 
subsidences  and  decantations  in  the  manner  just  described. 

In  this  way  there  is  removed  from  the  sediment,  on  the  one 
hand,  a  portion  of  silt  free  from  sand  and  dust,  and  on  the  other 
hand  a  portion  of  sand  free  from  silt.  Thus  is  obtained  a  second 
intermediate  portion  consisting  of  sand  and  silt,  but  less  in  amount 
than  the  first  and  containing  particles  of  diameters  much  more 
nearly  approaching  0.05  millimeter.  By  repeating  this  process 
a  few  times,  this  intermediate  portion  will  be  reduced  to  particles 
whose  diameters  are  very  near  0.05  millimeter  and  which  may 
be  divided  between  sand  and  silt,  according  to  judgment.  The 
amount  of  this  is  usually  very  small.  As  soon  as  portions  are 
separated,  which  the  microscope  shows  to  be  pure  sand  or  pure 
silt,  they  are  added  to  tha  chief  portions  of  these  grades  already 
obtained. 

The  same  process  is  applied  to  the  separation  of  silt  from 
dust.  When  all  the  silt  has  been  removed  from  the  dust  and  clay, 
the  turbid  water  containing  the  dust  and  clay  is  set  aside  and 
allowed  to  settle  in  a  cylindrical  vessel  for  twenty-four  hours. 
The  vessel  is  filled  to  a  height  of  200  millimeters.  According  to 
Hilgard,  the  separation  of  the  dust  from  clay  during  a  subsidence 
of  twenty-four  hours,  will  give  results  of  sufficient  accuracy, 
although  the  clay  then  remaining  suspended  will  not  be  entirely 


164  METHODS  OF  ANALYSIS 

free  from  measurable  fine  particles  up  to  0.001  or  0.002  millimeter 
diameter. 

Small  beakers  and  small  quantities  of  distilled  water  are  used 
at  first  for  the  decantations,  as  thus  the  duration  of  subsidence  is 
less  and  more  decantations  can  be  made  in  a  given  time  than  when 
larger  quantities  of  water  are  employed.  Beakers  of  about  100 
milliliters  capacity  are  convenient  for  the  coarser  grades,  but  it 
is  necessary  to  use  larger  vessels  for  the  fine  sediments  from  which 
turbid  water  accumulates  that  cannot  be  thrown  away,  as  may  be 
done  with  the  clear  water,  from  which  the  coarse  sediments  settle 
out  completely  in  a  short  time. 

It  is  best  to  keep  the  amount  of  water  as  small  as  possible  in 
working  out  the  dust  since  loss  is  incurred  in  using  too  large 
quantities. 

It  is  also  necessary  in  most  cases  to  subject  the  various  frac- 
tions obtained  during  elutriation,  to  careful  kneading  with  a  soft 
rubber  pestle  so  that  the  fine  lumps  of  clay  may  be  broken  up 
and  caused  to  remain  suspended  in  the  water.  This  treatment 
with  the  pestle  should  be  done  in  such  a  way  as  to  avoid  as  far 
as  possible  all  grinding  of  the  particles,  the  object  being  merely 
to  pulverize  the  minute  aggregations  of  clay  and  extremely  fine 
particles  which  always  form  on  drying  a  sample  of  soil  after 
removing  it  from  the  field. 

Measurement  of  the  Particles:  To  determine  the  size  of  par- 
ticles in  suspension,  a  small  glass  tubs  is  applied  to  the  surface 
of  the  liquid  in  such  a  way  as  to  take  up  a  single  drop  which  is 
transferred  to  a  glass  slide.  This  drop  will  contain  the  smallest 
particles  in  the  liquid. 

To  obtain  a  sample  of  the  coarsest  particles,  the  liquid  is 
allowed  to  stand  long  enough  to  form  a  very  slight  sediment,  and 
a  portion  of  this  sediment  is  collected  with  a  glass  tube. 

To  determine  the  diameter  of  the  particles  in  a  sediment,  it 
is  stirred  vigorously  with  a  little  water  and  the  pipette  at  once 
applied  to  the  surface  of  the  water.  On  decanting  the  greater 
part  of  the  sediment,  the  large  particles  remain  at  the  bottom  of 
the  beaker  and  may  be  easily  examined. 

Time:  The  time  required  to  make  the  separations,  above 
described,  is  about  two  hours  for  each,  so  that  an  analysis  includ- 
ing the  siftings,  is  made  in  five  or  six  hours,  exclusive  of  the  time 
necessary  for  collecting  the  dust  and  separating  the  clay,  for  which 
a  subsidence  of  24  hours  is  allowed. 


xxii.    SOIL  165 

\\'<iyhin(j  the  Xr(ii»i<nls:  The  sediments  are  prepared  for 
\\  i  i^liinu  by  allowing  them  to  subside  completely,  decanting  the 
clear  water  as  fai-  as  possible,  rinsing  them  into  a  weighed  platinum 
disli  and  igniting.  The  dish  is  cooled  in  a  desiccator,  and  the  ig- 
nited sediments  are  generally  very  hygroscopic. 

Effect  of  Boiling:  The  analyses  show  a  very  decided  increase 
in  the  particles  smaller  than  0.01  millimeter  diameter  at  the  ex- 
pense of  coarser  particles  as  the  result  of  boiling.  The  surfaces 
of  the  coarser  particles  are  seen  to  be  polished  and  of  a  lighter 
color  than  those  not  boiled.  The  surfaces  of  the  unboiled  par- 
ticles are  coated  with  a  film  of  fine  material  probably  cemented  to 
them  by  clay.  When  these  coarse  particles  which  have  not  been 
boiled,  are  violently  stirred  with  water  for  a  short  time,  no  fine 
particles  are  detached  from  them;  and  a  careful  examination 
under  the  microscope  fails  to  reveal  in  any  of  the  sediments  more 
than  an  occasional  grain  exceeding  the  0.05  millimeter  limit  by 
so  much  as  0.01  millimeter,  or  the  0.01  limit  by  as  much  as  0.005 
millimeter.  It  would,  therefore,  appear  that  these  small  particles 
thus  set  free  by  long  boiling  are  really  a  part  of  the  larger  ones 
and  should  be  treated  as  such  in  a  mechanical  analysis  of  these 
soils. 

9.     WATER  CAPACITY 

The  capacity  of  soil  to  take  up  water  by  capillary  action  is 
called  the  water  capacity.  This  varies  with  the  composition  and 

ially  with  the  mechanical  fineness  of  the  soil.  In  the  field 
there  are  other  influences,  such  as  the  manner  in  which  the  soil 
is  deposited,  the  height  of  the  ground  and  water,  and  other 
conditions. 

As  the  laboratory  test  cannot  imitate  all  these  conditions,  it 
i>i  only  of  relative  value. 

For  this  determination  a  Hilgard  "sieve  cylinder,"  which 
can  be  obtained  from  dealers  in  chemical  apparatus,  is  used.  It 
is  a  metal  cylinder,  open  at  the  top  and  closed  at  the  bottom  by 
a  fine  wn  The  cylinder  rests  in  a  ring  2  cm  high  provided 

at  the  sides  with  holes  which  allow  free  access  of  water  when 
immersed  in  a  beaker  containing  water.  The  wire  screeen  is  cov- 
»-ivd  inside  with  a  fine,  circular  linen  cloth.  The  cylinder  is  16 
cm  deep  x  4  cm  in  diameter,  so  that  its  contents  amount  to  200 
cubic  centimeters. 


166  METHODS  OP  ANALYSIS 

Before  the  test  moisten  the  linen  cloth,  and  weigh  the  appara- 
tus together  with  a  small  porcelain  dish  in  which  it  stands.  Then 
fill  the  cylinder  up  to  the  rim  with  the  air-dry  soil,  adding  it 
gradually  with  continual  shaking  until  no  further  settling  is 
noticeable.  Then  level  with  a  spatula  and  weigh  again.  Place 
the  cylinder  in  a  good  sized  beaker,  containing  enough  water  at 
room  temperature  to  submerge  the  sieve  bottom  of  the  cylinder 
to  the  -extent  of  5  to  10  millimeters,  and  cover  the  entire  apparatus 
with  a  glass  bell  jar  to  prevent  evaporation.  The  time  required 
to  reach  the  maximum  water  absorption  will  vary  with  the  nature 
of  the  soil.  As  soon  as  moisture  appears  at  the  surface,  take  out 
the  cylinder,  allow  it  to  drain  for  a  few  moments,  wipe  the  outside, 
place  it  in  the  porcelain  dish  originally  used,  and  weigh.  Put 
the  cylinder  back  in  the  water  for  some  time  and  weigh  again, 
repeating  this  procedure  until  the  weight  is  constant,  or  nearly 
so.  Calculate  the  increase  in  weight  as  the  percentage  on  the 
weight  of  the  air-dry  soil. 


10.     STATEMENT  OF  ANALYSIS 

Calculate  all  the  results  of  the  chemical  analysis  as  percent- 
ages of  the  soil  dried  to  constant  weight  at  the  temperature  of 
boiling  water,  and  report  in  the  order  given.  Under  "physical 
analysis"  express  the  results  as  percentages  on  the  air-dry  soil. 

CHEMICAL  ANALYSIS 

%  on  Moisture- 
free  Soil 
Insoluble  residue 
Lime   (CaO) 
Carbon  dioxide  (CO,) 
Potash  (K20) 
Soda  (Na20) 

Iron  and  aluminum  oxides  (Fe203  &  A1203) 
Manganese  oxide  (Mn804) 
Phosphoric  acid    (P203) 
Sulphuric  acid  (S03) 
Volatile  matter 
Humus 

Total  nitrogen 
Water  soluble 


xxn.    SOIL  167 

PHYSICAL  ANALYSIS 

%  on  Air- 
Dried  Soil 
Hygroscopic  moisture 

Water  capacity 

Temperature  of •  absorption  (°C.) 

Coarse  sand.  1.0  — 0.5  mm 

Medium  sand,  0.5  — 0.25  mm. 

Fine  sand,  0.25—0.05  mm 

Silt,  0.05—0.01  mm 

Dust,  less  than  0.01  mm 


XXIII.     APPARATUS 

In  addition  to  the  data  given  in  this  chapter,  many  articles 
and  arrangements  of  apparatus  will  be  found  described  in  con- 
nection with  the  directions  for  particular  determinations. 

1.  BALANCES 

Analytical  balances  of  the  standard  grade  and  sensibility 
should  be  employed.  Pulp  balances  should  be  rugged  in  con- 
struction and  sensible  to  2  milligrams. 

2.  BEET  RASP 

A  rasp  of  the  Keil-Dolle  type  is  employed  for  the  samples 
handled  in  the  beet  laboratory.  This  rasp  removes  a  true  radial 
segment  from  each  beet  and  at  the  same  time  reduces  it  to  a  very 
fine  pulp  suitable  for  analysis  by  the  cold  water  method.  It  has 
been  found  by  a  great  number  of  tests  that  the  portion  of  the 
beet  removed  by  a  rasp  of  this  kind  is  on  the  average  a  very  accu- 
rate sample  of  the  whole  beet.  Special  directions  regarding  the 
care  and  use  of  this  rasp  will  be  found  in  detail  in  Chap.  XII, 
2  and  3. 

3.  CAPSULES  AND  COVERS  FOR  ANALYSIS  OF  BEETS 

Metal  cups,  so-called  "capsules,"  are  employed  in  the  deter- 
mination of  sugar  in  the  beet  by  the  cold  water  digestion  method. 
They  are  all  adjusted  to  the  same  tare  by  grinding  or  by  adding 
solder,  and  should  be  made  of  Monel  metal  (or  nickel),  as  other 
common  metals  will  be  attacked  by  the  lead  acetate  solution  and 
the  tare  will,  as  a  result,  change  rapidly.  The  capsules  should 
be  about  3  in.  dia.  x  3  in.  high,  or  of  about  350  ml  capacity. 

The  cover  consists  of  an  aluminum  disc,  4^  in.  dia.  x  %  in. 
thick,  which  has  a  hole  1-%  in.  in  diameter  at  the  center,  and  over 


XXIII.       APPARATUS  169 

it  is  stretched  a  rubber  envelope.  When  the  cover  is  placed  on 
the  capsule,  the  rubber  is  pressed  with  the  thumbs  downward 
through  the  central  opening.  On  releasing  the  pressure  a  slight 
vacuum  is  created,  which  holds  the  cover  on  firmly ;  this  makes  an 
air-tight  joint  which  prevents  evaporation,  and  also  loss  of  the 
contents  if  the  capsule  is  accidentally  knocked  over. 

4.  CARBONATOR 

For  carbonating  saccharate,  a  carbonator  of  familiar  construc- 
tion is  employed.  It  should  have  means  for  injecting  steam  and 
carbon  dioxide  gas,  which,  for  convenience  and  to  avoid  local  over- 
heating of  the  juice,  should  preferably  be  introduced  through 
connections  at  the  bottom  rather  than  through  pipes  running 
down  through  the  liquid. 

5.     COOLER 

The  laboratory  cooler  is  a  working  model  of  the  factory  coolers. 
No  particular  description  is  necessary.  See  section  17  for  the 
speeds  of  the  various  pulleys.  Care  should  be  taken  to  avoid  wet- 
ting the  bolter  screen.  When  it  becomes  stopped  up,  the  bolter 
should  be  removed  and  the  screen  cleaned  by  washing  it  first 
with  hydrochloric  acid,  then  with  water,  and  drying  in  a  warm 
place. 

6.     DISHES  FOR  MOISTURE  DETERMINATIONS 

Aluminum  dishes  2  in.  dia.  x  I1/-.*  in.  high  should  be  employed 
for  dry  substance  determinations  in  general ;  for  dried  pulp  alu- 
minum dishes  3  in.  dia.  x  •"»<•  in.  high  should  be  used.  Each  dish 
should  have  a  loosely  fitting  aluminum  cover  provided  with  a 
knob  of  the  same  material,  and  both  the  dish  and  the  cover  should 
be  numbered  with  a  die. 

7.     DRYING  OVENS 

Electric  ovens,  even  those  of  the  best  make,  fall  far  short  of 
the  requirement  of  uniform  temperature,  as  one  will  commonly 
find  variations  of  10 — 20°  not  only  at  different  levels  but  also  at 
different  points  on  the  same  shelf.  They  are  accordingly  not  to 
be  recommended  except  possibly  for  drying  empty  dishes. 


170  METHODS  OF  ANALYSIS 

A  double  walled  oven  of  suitable  construction,  the  jacket 
of  which  is  filled  with  a  boiling  glycerin  solution,  will  give  a  tem- 
perature which  is  uniform  within  2  to  3  degrees  in  all  parts  of 
the  oven,  provided  the  dishes  are  placed  on  shelves  and  not  directly 
on  the  bottom  of  the  oven.  This  type  of  oven  is  accordingly 
recommended  for  dry  substance  determinations. 

The  glycerin  solution  should  be  of  such  a  strength  that  the 
required  temperature  (commonly  100 — 105°)  will  be  maintained 
in  the  interior  of  the  oven.  For  630  mm  barometric  pressure 
(5000  feet  elevation)  a  mixture  of  about  3  parts  of  glycerin  and 
1  part  of  water,  which  has  a  density  of  about  42°  Brix,  will  give 
approximately  the  desired  concentration.  The  boiling  point  of 
the  glycerin  solution  should  be  kept  constant  by  means  of  a  reflux 
condenser.  It  will  occasionally  be  necessary  to  add  a  little  water 
ta  replace  the  water  which  is  lost  by  evaporation  and  is  not  caught 
by  the  condenser. 

8.  EVAPORATOR 

An  open  evaporator  heated  by  a  steam  chamber  at  the  bot- 
tom is  the  type  of  laboratory  evaporator  recommended  and 
commonly  employed. 

9.     GRINDING  MACHINERY 

For  grinding  cossettes  employ  an  Enterprise  Meat  Chopper 
No.  41,  with  a  plate  containing  %  inch  perforations,  and  running 
at  the  rate  of  300  R.  P.  M.  For  grinding  pulp  use  a  second 
machine  of  the  same  description. 

For  preparing  for  analysis  samples  of  material  such  as  lime- 
stone, boiler  house  ashes,  etc.,  a  combination  of  a  jaw  crusher  with 
a  disc  pulverizer  is  very  satisfactory.  Material  of  great  hardness, 
such  as  coke,  must  not  be  ground  in  a  disc  pulverizer  on  account 
of  the  contamination  which  will  affect  the  sample. 

Large  samples  of  coal  are  ground  in  a  pebble  mill,  by  means 
of  which  they  may  be  ground  to  the  necessary  fineness  during  a 
long  period  of  time  without  important  loss  of  moisture.  The  mill 
for  this  purpose  has  a  cast  iron  jar  18  x  18Vi>  in.,  which  should 
revolve  at  the  rate  of  40 — 50  R.  P.  M.,  and  should  contain  100 
pounds  of  smooth,  best  grade  flint  pebbles.  Inspect  the  contents 
occasionally  for  the  presence  of  broken  pebbles,  which  should  be 
removed  and  discarded. 


XXIII.       APPARATUS  171 

10..   HYDROMETERS. 

Laboratory  Brix  hydrometers  should  have  a  total  length  of 
about  12  inches  and  a  range  of  6°  Brix  each,  starting  at  0 — 6°  and 
up  to  and  including  72 — 78°.  The  scale  should  be  graduated  in 
one-tenths  of  one  degree  Brix  and  should  cover  a  distance  of  not 
less  than  41/4  inches  on  the  stem.  Baume  hydrometers,  for  testing 
molasses,  should  have  enclosed  thermometers,  should  have  ranges 
of  30 — 40  and  40 — 50  degrees  Baume,  a  total  length  of  13  inches, 
a  scale  length  of  4%  inches,  and  should  be  graduated  in  one-tenths 
of  one  degree  Baume.  The  standard  temperature  for  both  Brix 
and  Baume  hydrometers  is  20°.  All  laboratory  hydrometers  must 
be  verified  as  described  in  Chap.  XXIV,  3,  and  any  more  than 
0.1  degree  in  error  at  any  point  must  be  rejected  or  readjusted. 

11.  HYDROMETER  JARS 

The  hydrometer  jars  used  with  the  laboratory  Brix  hydro- 
meters should  be  12  inches  long  and  2  inches  in  diameter  (inside 
dimensions) . 

12.  PLATINUM,  CARE  OF 

In  making  ignitions  or  fusions  in  platinum  vessels  by  means 
of  the  Bunsen  burner,  only  the  upper  non-luminous  cone  of  the 
flame  should  be  employed,  and  not  the  inner  cone,  nor  should  a 
smoky  flame  be  used,  as  the  action  of  a  flame  containing  free  car- 
bon will  result  in  the  formation  of  a  carbide  of  platinum,  causing 
the  metal  to  become  brittle.  At  the  best  a  tarnish  will  gradually 
develop,  which  should  be  removed  by  gentle  rubbing  with  moist 
sea  sand,  the  grains  of  which  are  rounded  and  do  not  scratch  the 
metal.  Platinum  ware  should  be  kept  polished  in  this  manner, 
as  the  tarnish  increases  more  rapidly  upon  already  tarnished 
surface*,  and  will  eventually  lead  to  corrosion  and  cracking. 
Platinum  surfaces  may  also  be  cleansed  by  fusing  borax  upon 
them  and  by  digestion  with  nitric  acid. 

The  following  precautions  should  be  observed  in  the  use  of 
platinum  utensils: 

(a)  Platinum  is  insoluble  in  any  single  acid,  but  is  readily 
Milublr  in  a  mixture  of  hydrochloric  and  nitric  acids  (aqua  regia). 

(b)  Fusions  in  which  the  hydroxides  of  sodium,  potassium, 
or  barium  are  used  should  not  be  performed  in  platinum. 


172  METHODS  OF  ANALYSIS 

(c)  All   metals   which   may   be   reduced   in   a   fusion — espe- 
cially  compounds  of  lead,   bismuth,   tin,   and  other  metals  easily 
reduced  and  melted — and  all  metallic  compounds  with  reducing 
agents  form  fusible  alloys  with  ignited  platinum.     Mercury,  lead, 
bismuth,  tin,  antimony,  zinc,  etc.,  are  liable  to  be  rapidly  reduced 
and  immediately  melt  away  platinum  in  contact  with  them. 

(d)  Free  chlorine  and  bromine  attack  platinum  at  ordinary 
temperature,   and   free  sulphur,   phosphorus,   arsenic,   and   iodine 
attack   ignited    platinum.      Operations   in    which    these    elements 
are  set  free   should  not  be  performed  in   platinum.     Hence   the 
fusion    of    sulphides,    sulphates,    and    phosphates    with    reducing 
agents  should  be  avoided,  and  care  should  be  exercised  in  igniting 
phosphates  in  the  presence  of  carbon  from  burnt  filters. 

13.     POLARISCOPES  (SACCHARIMETERS) 

No  detailed  explanation  of  the  theory  and  construction  of 
polariscopes  will  be  given  here,  as  this  subject  will  be  found  treated 
at  length  in  the  various  textbooks.  See  for  example  Browne's 
"Handbook  of  Sugar  Analysis"  and  Circular  44,  " Polarimetry, " 
of  the  Bureau  of  Standards.  While  the  sugar  chemist  is  advised 
to  let  the  optical  parts  of  the  instrument  alone  as  far  as  possible, 
it  is  desirable  that  he  have  a  full  understanding  of  the  principles 
relating  to  the  construction  and  use  of  saccharimeters.  A  few 
points  are  discussed  below  to  which  it  is  desired  to  direct  special 
attention. 

(a)  SPECIFICATIONS 

The  type  of  polariscope  to  be  preferred  for  general  laboratory 
control  work  is  the  double  field,  single  compensation,  400  mm  tube 
length,  mounted  on  a  trestle  support.  The  *report  of  the  com- 
mittee of  the  American  Chemical  Society  covers  in  great  detail 
the  desirable  features  of  a  commercial  saccharimeter. 

(b)  SACCHARIMETRIC  SCALE  AND  NORMAL  WEIGHT 

The  100  degree  point  is  defined  as  the  scale  reading  given 
by  the  polarization  of  the  "normal  weight"  of  pure  sucrose, 
weighed  in  air  with  brass  weights,  and  dissolved  in  water  and 
made  up  to  a  volume  of  100  ml  at  20°,  the  temperature  of  the 
solution  and  of  the  optical  parts  of  the  instrument  during  polariza- 
tion being  20°.  The  "normal  weight"  at  present  most  commonly 
in  use,  and  the  standard  employed  in  this  book,  is  26  grams. 
See  also  Chap.  XXIV,  7  (a). 


*Jour.  Ind.  &  Eng.  Chem,  12,  440. 


XXIII.       APPARATUS  173 

(c)  VERIFICATION  OF  SCALE 

See  Chap.  XXIV,  7  (a).  When  the  accuracy  of  the  scale 
has  once  been  established,  it  suffices  for  ordinary  purposes  to  keep 
the  instrument  in  adjustment  at  the  zero  point  and  to  check  it 
occasionally  with  standard  quartz  plates.  The  Chief  or  Assistant 
Chemist  should  check  the  setting  of  the  zero  point  at  least  twice 
a  shift,  and  oftener  if  it  appears  desirable. 

(d)  EFFECT  OF  TEMPERATURE  ON  POLARIZATION 

The  polarization  of  a  pure  .sugar  solution  decreases  by  about 
.03%  for  each  degree  increase  in  temperature.  If  the  solution, 
when  made  up  to  volume  and  polarized  at  a  given  temperature  (t), 
shows  a  polarization  of  St,  the  polarization  of  20°  (S20)  is  given 
by  the  following  formula : 

S2ft  =  St+  .0003  St(t— 20) 

If  the  solution  is  made  up  to  volume  at  20°  but  is  polarized  in  a 
glass  tube  at  some  other  temperature,  the  temperature  coefficient 
in  the  formula  becomes  .0006  instead  of  .0003 ;  plainly  this  pro- 
cedure will  only  increase  the  liability  of  error.  On  the  other  hand 
if  the  solution  is  both  made  up  and  polarized  at  20°  while  the 
polariscope  is  at  some  other  temperature,  the  temperature  coef- 
ficient is  that  for  the  instrument  alone,  which  is  given  by  Schonrock 
as  ..000148  for  the  ordinary  quartz  wedge  saccharimeter  with 
nickelin  scale,  and  as  .000138  if  the  scale  is  of  glass. 

In  the  case  of  an  impure  sugar  solution,  the  temperature 
coefficient  is  equal  to  the  algebraic  sum  of  the  various  influences, 
including  those  of  the  associated  impurities,  and  may  be  more  or 
less  than  the  value  for  pure  sugar,  which  it  is  therefore  unsafe  to 
apply  in  the  polarization  of  an  impure  solution.  According  to 
*Browne  the  temperature  coefficient  for  the  direct  polarization 
of  beet  molasses  is  almost  negligible,  and  for  raw  beet  sugars  is 
about  the  same  as  for  pure  sucrose. 

While  work  of  the  highest  precision  demands  the  use  of  a 
constant  temperature  room  which  can  be  kept  at  exactly  20°, 
sufficiently  accurate  results  for  ordinary  control  work  are  obtained 
by  making  up  and  polarizing  the  solutions  at  room  temperature. 
It  follows,  however,  that  the  room  temperature  should  be  kept 
as  close  to  20°  as  the  heating  and  ventilating  arrangements  will 


*Jour.  Ind.  &  Eng.  Chem.,  1,  567. 


174  METHODS  OF  ANALYSIS 

permit.  The  accuracy  can  be  increased  by  making  up  and  polariz- 
ing the  solutions  at  20°,  in  which  case,  if  the  room  temperature 
is  not  .20°,  the  only  correction  is  that  due  to  the  temperature 
coefficient  of  the  saccharimeter,  which,  as  given  above,  is  not  great 
and  is  a  fairly  definite  figure  for  any  single  instrument;  this  pro- 
cedure is  not  adapted  for  a  large  volume  of  work  but  is  applicable 
in  special  cases. 

As  the  specific  rotation  of  inverted  solutions  varies  greatly 
with  the  temperature,  all  such  solutions  must  be  made  up  and 
polarized  at  exactly  20°. 

(e)  INSTALLATION 

The  saccharimeter  should  be  installed  in  a  "polariscope  box" 
of  the  customary  construction,  which  should  have  a  partition  at 
the  rear  with  a  small  hole  at  the  proper  height  for  illuminating 
the  instrument  without  allowing  bright  light  to  strike  the  ob- 
server's eye,  should  be  painted  a  dead  black  on  the  inside,  and 
should  be  provided  with  a  dark  curtain  at  the  front,  open  end 
to  exclude  outside  light.  The  location  should  be  free  from  excessive 
heat  or  cold  drafts,  and  as  little  subject  as  possible  to  undue  varia- 
tions in  temperature. 

( f )  ILLUMINATION 

A  Mazda  C  stereopticon  lamp  is  the  most  satisfactory  source 
of  illumination.  A  finely  frosted  glass  plate  should  be  fastened 
so  as  to  cover  the  opening  in  the  partition  of  the  polariscope  box 
and  the  lamp  should  be  placed  as  close  behind  this  as  possible. 
The  lamp  should  be  clamped  on  a  firm  bracket,  or  support,  which 
has  means  for  vertical  and  lateral  adjustment.  To  avoid  shifting 
of  the  zero  point  it  is  essential  that  the  instrument  be  kept  in 
alignment  with  the  source  of  illumination,  and  for  this  purpose 
not  only  should  the  lamp  be  firmly  mounted  but  the  polariscope 
should  also  be  kept  in  a  fixed  position  by  means  of  bolts  or  strips 
of  wood,  etc.  Particular  care  should  be  taken  to  adjust  the  position 
of  the  lamp  so  that  the  brightest  portion  is  in  alignment  with  the 
optical  axis  of  the  saccharimeter. 

Electric  lamps  will  darken  with  use,  and,  when  this  has  taken 
place  to  such  an  extent  that  the  illumination  is  insufficient,  they 
should  be  discarded. 

The  instrument  should  never  be  placed  so  close  to  the  source 
of  light  as  to  permit  overheating  to  take  place  and  hence  possible 


xxra.    APPARATUS  175 

» 

damage  to  the  optical  parts.  The  rule  is  that  the  polariseope 
should  be  placed  at  such  a  distance  from  the  source  of  light  that 
the  image  of  the  latter  is  clearly  defined  upon  the  analyzer  dia- 
phragm; this  is  best  accomplished  by  fastening  a  needle  or  other 
sharp  pointed  object  at  the  source  of  light  (the  frosted  glass  plate) 
and  changing  the  position  of  the  instrument  until  a  clear  inverted 
image  of  the  point  is  obtained  upon  a  piece  of  white  paper  placed 
before  the  analyzer  diaphragm.  The  distance  of  Schmidt  & 
Haensch  instruments  from  the  source  of  light  is  given  by  the 
manufacturers  as  150  millimeters  ;  it  is  also  directed  by  them  that, 
in  the  case  of  their  1909  model  instrument  provided  with  the 
"Blendrohr,"  when  the  light  filter  is  in  place  the  sleeve  containing 
the  condensing  lens  must  be  drawn  out  to  the  extent  of  8.9  mm, 
i.  e.,  up  to  the  engraved  mark,  and  the  distance  of  the  condensing 
lens  from  the  source  of  light  must  then  be  adjusted  to  150  mm. 

(g)     LIGHT  FILTER 

It  is  important  that  a  light  filter  be  constantly  used.  A  com- 
mon arrangement  consists  of  a  cell  containing  a  solution  of  potas- 
sium dichromate.  If  "a"  is  the  length  of  the  cell  in  centimeters 
and  "b"  is  the  percentage  strength  of  the  dichromate  solution, 
the  proper  value  of  the  latter  is  found  from  the  formula 


For  example,  if  the  cell  is  3  cm  long,  a  3%  solution  must  be  used. 

In  some  instruments  a  glass  plate  is  employed  as  a  light  filter, 
and  in  one  make  of  saccharimeter  means  are  provided  by  which  a 
light  filter  of  this  kind  may  readily  be  thrown  in  or  out  of  the 
optical  system;  in  this  case  readings  should  always  be  made  with 
the  light  filter  in  place  except  in  the  case  of  a  very  dark  solution 
which  contains  enough  coloring  matter  to  serve  as  its  own  light 
filter. 

(h)     TUBES  AND  COVER  GLASSES 

In  filling  a  tube  for  polarization,  it  is  customary  to  rinse  it 
first  two  or  three  times  with  the  solution,  then  to  fill  it,  put  the 
cover  glass  in  place,  and  attach  the  cap.  The  caps  should  not  be 
screwed  on  too  tight,  as  the  strain  on  the  glass  thereby  created 
may  cause  optical  rotation. 

Metal  tubes  are  satisfactory  for  ordinary  work,  but  they 
should  be  examined  and  tested  frequently  to  see  that  they  do  not 


176  METHODS  OF  ANALYSIS 

become  bent.     See   Chap.   XXIV,   7    (b).     Glass  tubes   are   free 
from  this  drawback. 

Cover  glasses  must  be  kept  clean  and  dry.  It  is  impossible 
to  do  accurate  work  with  smeary  cover  glasses.  Scratched  glasses 
should  be  discarded. 

(i)     CARE  AND  ADJUSTMENT  OF  POLARISCOPES 

As  an  almost  inflexible  rule,  the  adjusting  of  the  polariscope 
should  be  limited  to  the  setting  of  the  zero  point,  as  mentioned 
under  (b),  and  to  careful  cleaning  of  the  splash  glasses  and  ex- 
posed lenses. 

The  half-shadow  angle,  which  is  fixed,  or  not  readily  adjust- 
able, in  most  commercial  saccharimeters,  represents  a  compromise 
between  maximum  sensibility  and  sufficient  illumination  for  polar- 
izing dark  solutions;  a  decrease  of  the  half-shadow  angle  results 
in  increased  sensibility  but  in  decreased  illumination.  It  varies 
from  about  6  to  9  angular  degrees  in  most  commercial  instruments, 
and  may  be  determined  by  measuring  the  interval  in  sugar  degrees 
between  the  points  of  maximum  light  extinction  on  each  side  of 
the  zero  point,  and  then  multiplying  by  .3466  to  convert  to  angular 
degrees.  If  it  is  necessary  to  change  the  half -shadow  angle,  this 
may  be  do>ne,  in  instruments  provided  with  the  Lippich  polarizing 
system,  by  rotating  the  large  polarizing  Nicol  to  a  new  position, 
and  then,  with  the  quartz  wedge  scale  set  at  zero,  rotating  the 
analyzer  till  the  two  halves  of  the  field  show  equality  of  brightness, 
or  very  nearly  so;  the  zero  point  may  then  be  adjusted,  if  neces- 
sary, by  the  usual  arrangement  for  changing  the  position  of  the 
vernier. 

14.     PRESSES 

Hydraulic  presses,  operated  at  a  standard  pressure,  must  be 
employed  to  obtain  the  juice  from  ground  beets  or  cossettes  for 
the  determination  of  apparent  purity.  The  standard  pressure 
to  be  used  upon  the  ground  material  is  240  Ibs.  per  sq.  in.,  and 
the  corresponding  gage  pressure  for  different  types  of  presses  is 
calculated  as  follows: 

Let  a  =  diameter  of  ram  in  inches 

b  =  inside  diameter  of  basket  in  inches  (if  round) 
c  =.area  of  basket  in  square  indies  (if  square  or  rect- 
angular) 


XXIII.       APPARATUS  177 

P  =  gage  pressure  in  pounds  per  square  inch. 

240  Ir                    306  c 
Then  I  = —  or  P  = ; — 

a-  M  ~ 

<» 

E.  g.,  if  a  =  4  and  b  =  10,  P  =  1500.  In  obtaining  the  dimen- 
sions, measure  the  rani  at  the  eup  leather  across  the  entire  effective 
surface. 

As  the  percentage  of  sugar  in  the  juice  obtained  from  pulp 
at  different  pressures  does  not  vary  noticeably,  a  hand  operated 
lard  press  is  satisfactory  for  this  purpose. 

15.     RADIATOR  FOR  VOLATILIZING  LIQUIDS  AND 

SOLIDS 

The  radiator  described  by  Hillebrand  in  U.  S.  Geological 
Survey  Bulletin  700,  "The  Analysis  of  Silicate  and  Carbonate 
Rocks,"  page  33,  is  frequently  recommended  in  this  book  and  will 
be  found  greatly  superior  to  the  hot  plate  or  sand  bath  for  evapo- 
rating such  liquids  as  sulphuric  acid  rapidly  without  loss  by 
decrepitation. 

16.  REFRACTOMETERS 

The  refractometer  used  in  sugar  work  is  of  the  Abbe  type 
and  is  provided  with  a  dry  substance  scale  based  on  the  Deter- 
minations of  Schonrock.  The  standard  temperature  for  the  use 
of  the  instrument  is  20°.  No  special  directions  for  the  use  of  the 
instrument  beyond  those  given  in  Chap.  I,  2  (b)  and  XXIV,  8, 
are  probably  necessary. 

17.     SPEEDS  OF  LABORATORY  MACHINERY 

The  following  resume  of  the  speeds  at  which  +he  laboratory 
machinery  should  be  operated  will  be  found  convenient  for 
reference : 

R,  P.  M. 

Beet   Rasp    (Keil  disc) 600-700 

Case  Crusher     450-500 

Cooler,  Laboratory — 

Propeller    200 

Bolter    40 

Conveyor  (auger  type) 35 


*Bureau  of  Standards  Circular  44,  "Polarimetry,"  2nd  ed.,  p.  134. 


178  METHODS  OF  ANALYSIS 

R.  P.  M. 
Curtis  Vacuum  Pump  and  Air  Compressor1...        250   (at  least) 

Enterprise  Meat  Chopper  No.  41 300 

Hydraulic  Press    (Hydraulic   Press  Mfg.    Co.), 

countershaft    80 

Her    Disc   Pulverizer 350-450 

McCool  Disc  Pulverizer  • 300 

Pebble  Mill    (jar  18y2  x  18  in.) 40-50 

Samson    Crusher    .  500 


18.     THERMOMETERS 

The  Centigrade  scale  alone  should  be  employed.  The  only 
exception  to  this  is  the  use  of  the  Fahrenheit  scale  in  recording 
boiler  house  temperatures.  Unless  otherwise  expressly  stated,  all 
temperatures  in  this  book  are  in  degrees  Centigrade.  For  deter- 
mining the  temperature  correction  in  the  apparent  purity  deter- 
mination, a  small  floating  thermometer,  with  enclosed  paper  scale, 
of  0 — 30°  range,  is  recommended.  Clerget  thermometers,  for  inver- 
sion readings,  must  be  of  special  construction  and  accurate  within 
0.1°  at  the  20°  point. 

19.     VOLUMETRIC  APPARATUS 

All  flasks,  burettes,  pipettes,  and  other  volumetric  apparatus 
should  be  standardized  as  described  in  Chap.  XXIV,  2.  "Sugar" 
flasks  should  be  made  heavier  than  the  ordinary  standard  to  save 
breakage,  but  the  100  ml  flasks  used  for  inversions  should  have 
sufficiently  thin  walls  so  that  the  solutions  will  reach  the  neces- 
sary temperature  in  the  time  required. 


XXIV.     STANDARDIZATION  AND  VERIFICATION  OF 
LABORATORY  APPARATUS 

1.     GENERAL 

All  kinds  of  laboratory  apparatus  used  for  quantitative 
measurements  must  be  carefully  verified  before  use.  Sacchari- 
meters,  refractometers,  and  weights  should  be  checked  at  frequent 
intervals.  It  should  also  be  remembered  that  glass  apparatus  will 
gradually  undergo  a  slight  change  in  capacity  until  it  has  had 
several  years'  seasoning. 

Tolerances:  The  "specifications  for  laboratory  apparatus" 
give  the  limits  of  error  allowable  for  each  class  of  apparatus. 


2.     VOLUMETRIC  APPARATUS 

(a)     GENERAL 

Units  of  Capacity:  The  liter,  defined  as  the  volume  occupied 
by  a  quantity  of  pure  water  at  4°  C.  having  a  mass  of  one  kilo- 
gram, and  the  one-thousandth  part  of  the  liter,  called  the  milli- 
liter  (cubic  centimeter),  are  the  units  of  capacity. 

Standard  Temperature:  The  standard  temperature  for  the 
use  of  glass  volumetric  apparatus  is  20°  C. 

The  apparent  weight  in  air  of  one  liter  of  water  at  20°  C. 
(weighed  with  brass  weights  in  air  at  76  cm  barometric  pressure 
and  50%  relative  humidity)  is  997.18  grams.  At  63  cm  barometric 
pressure  (5,000  feet  elevation)  the  apparent  weight  is  997.36 
grams;  the  difference  is  so  small  that  it  may  be  disregarded  in 
ordinary  work. 

Tables  35 — 47  of  Bureau  of  Standards  Circular  19,  5th  ed., 
"Standard  Density  and  Volumetric  Tables,"  will  be  found  useful 
in  calibrating  volumetric  glassware. 


180  METHODS  OF  ANALYSIS 

Reading:  In  adjusting  the  meniscus  to  the  graduation  mark, 
the  lowest  point  of  the  curve  when  viewed  against  a  white  surface 
should  just  touch  the  level  of  the  mark. 

(b)  FLASKS 

Clean  and  dry  the  flask  thoroughly,  and  standardize  by  one 
of  the  following  methods : 

(1)  Weigh  the  flask  first  empty  and  then  filled  with  recently 
boiled,  distilled  water.     Both  the  flask  and  the  water  should  be 
at  room  temperature,  and  the  temperature  of  the  water  should  be 
accurately    determined    with    a    thermometer.      Adjust    the    flask 
according  to  the  tables  in  Bureau  of  Standards  Circular  19.     For 
example,  a  100  ml  flask  must  be  graduated  to  hold  100  —  .340  = 
99.66  grams  of  water  at  23°  C.     (See  Table  38  of  the  Circular) 

(2)  Fill  the  flask  from   a  standardized  pipette   or  burette, 
using  clean  water  at  room  temperature.     The  pipette  or  burette 
employed  for  this  purpose  should  be  carefully  standardized  under 
definite  conditions  of  manipulation  and  used  under  the  same  con- 
ditions.    If  the  outflow  is  sufficiently  ^restricted  by  the  size   of 
the  orifice  in  the  tip,  no  period  of  drainage  need  be  allowed ;  other- 
wise a  definite  period  of  drainage,   e.   g.,   15  seconds,  should  be 
used.     In  either  case  the  water  remaining  in  the  tip  should  not 
be  blown  out,  but  the  emptying  should  be  completed  by  t touching 
the  tip  to  the  wet  surface  of  the  receiving  vessel. 

(3')  Employ  a  flask  standardized  by  weight  as  under  (1). 
Fill  the  clean,  dry  flask  with  clean  mercury  at  room  temperature, 
and  transfer  the  latter  with  the  aid  of  a  small  funnel  to  the  flasks' 
of  the  same  capacity  to  be  tested  (previously  cleaned  and  dried). 
Return  the  mercury  occasionally  to  the  standard  flask  to  make 
sure  that  there  has  been  no -loss  or  alteration  in  volume  due  to 
change  of  temperature  in  handling.  This  method  ip«  convenient 
and  safe  only  for  flasks  of  small  capacity. 

( c )  PIPETTES 

Verify  pipettes  by  weighing  the  water  delivered.  Use  distilled 
water  at  room  temperature,  and  obtain  the  capacity  from  the  tables 
in  Bureau  of  Standards  Circular  19.  If  the  graduation  mark  is 
found  incorrect,  make  a  new  temporary  mark  and  test  again,  re- 


*See  Bureau  of  Standards  Circular  9,  8th  ed.,  p.  17,  "Testing  of  Glass 
Volumetric  Apparatus." 
tLoc.  cit.,  p.  26. 


XXIV.       STANDARDIZATION    OF    APPARATUS  181 

peat  ing  this  procedure  until  the  correct  point  for  the  graduation 
is  found. 

Pipettes  should  be  standardized  under  the  conditions  under 
which  they  are  to  he  used.  Pipettes  for  analytical  work  of  high 
precision  should  be  standardized  as  described  under  "Flasks"  (2). 
Pipettes  for  routine  sugar  laboratory  work  must  necessarily  have 
uo<;d  sized  orifices,  but  in  use  the  tip  is  immediately  touched  to 
the  wet  surface  of  the  receiving  vessel  to  complete  the  emptying, 
without  allowing  any  period  of  drainage. 

(d)  BURETTES  AND  AUTOMATIC  PIPETTES 

Burettes:  Calibrate  burettes  in  a  similar  manner  to  pipettes 
by  weighing  the  water  discharged.  Empty  them  slowly  and  check 
at  several  different  points  in  the  scale,  as  well  as  for  the  largest 
amount  which  they  will  deliver.  Burettes  may  also  be  verified 
by  connecting  them  with  a  ''standardizing  pipette"  by  means  of 
which  successive  portions  of  water  of  5  ml  each  can  be  drawn  off 
and  measured. 

M  insuring  Pipettes:  Check  measuring  pipettes,  so-called 
Mohr  pipettes,  in  a  similar  manner  to  burettes. 

Automatic  Pipettes:  The  177  ml  automatic  pipettes  should 
deliver  177  ml  of  water  within  an  accuracy  of  0.25  ml. 

Orsat  Burettes:  Check  Orsat  burettes  at  the  100  ml  point 
and  at  intermediate  points  up  to  about  the  35  ml  graduation  mark. 
If  the  ratios  of  the  smaller  capacities  to  the  total  capacity  are 
correct  the  burette  may  be  used  without  error,  even  if  the  measure- 
ments do  not  represent  true  milliliters. 

(e)  ETCHING  GRADUATION  MARKS 

Stopper  the  flask,  or  other  piece  of  glassware,  and  immerse 
the  neck  in  melted  paraffin.  After  the  paraffin  has  hardened  place 
the  flask  in  a  suitable  apparatus,  by  menus  of  which  it  can  be 
rotated  evenly  about  its  axis  and  the  graduation  can  be  marked 
by  a  stylus  attached  to  the  apparatus.  Then  dip  the  flask  in  a 
hydrofluoric  acid  mixture,  such  as  "Diamond  Ink."  After  a  few 
minutes  wash  off  the  acid  and  remove  the  paraffin  with  gasoline 
or  by  other  suitable  means.  The  graduation  mark  should  be  fine, 
exactly  perpendicular  to  the  axis,  and  should  appear  as  a  single 
^traijrht  line  when  viewed  without  parallax. 

Where  it  is  necessary  to  regraduate  a  flask  or  piece  of  volu- 
metric apparatus  which  already  has  an  incorrectly  placed  gradua- 


182  METHODS  OF  ANALYSIS 

tion  mark,  errors  due  to  confusion  of  the  two  marks  will  be  avoided 
by  the  use  of  a  *colored  mark  applied  as  follows:  Mix  ceramic 
green  728  D  (Roessler  &  Hasslacher  Chemical  Co.)  intimately 
with  a  vehicle  made  up  of  4  parts  of  copaiba  balsam,  1  part  of  clove 
oil,  and  1  part  of  lavender  oil,  using  just  enough  of  the  vehicle 
so  that  the  mixture  will  run  slowly  from  a  pen.  After  marking, 
heat  with  a  flame  the  region  where  the  mark  has  been  made  until 
the  color  begins  to  glow,  being  careful  not  to  heat  to  the  softening 
point  of  the  glass.  Allow  to  cool  a  little,  then  reheat  until  the 
markings,  not  the  glass,  again  begin  to  glow. 


3.     HYDROMETERS 

(a)  BRIX  HYDROMETERS,  GENERAL 

Standard  Temperature:  Brix  hydrometers  indicate,  in  a  solu- 
tion of  pure  sugar  at  20°,  the  direct  percentage  of  sugar.  The  limit 
of  error  at  any  point  on  the  scale  should  not  exceed  0.1°  Brix. 

Cleansing:  Wash  the  hydrometers  thoroughly  with  soap  and 
water,  rinse,  and  dry  with  a  clean  linen  cloth.  In  order  to  make 
the  liquid  adhere  readily,  dip  the  stems  in  strong  alcohol,  and  wipe 
immediately  with  a  soft,  clean,  linen  cloth. 

Points  to  be  Checked:  Check  at  least  two  points  on  every 
hydrometer,  one  near  each  end  of  the  scale,  and  preferably  an 
additional  point  at  the  middle. 

Test  Liquid:  Use  a  sulphuric  acid  solution  in  every  case  for 
the  test  liquid. 

(b)  PYCNOMETER  METHOD 

A  50  ml  pycnometer  of  the  Bureau  of  Chemistry  type  (E.  & 
A.  Cat.  No.  1086)  is  preferable.  First  determine  the  capacity  of 
the  pycnometer  by  weighing  it  empty,  and  filled  with  recently 
boiled,  distilled  water  at  20°.  Make  at  least  three  or  four  such 
determinations,  which  should  agree  closely.  Then  rinse  and  fill 
the  pycnometer  with  the  test  solution,  also  at  exactly  20°,  and 
weigh,  making  at  least  two  such  determinations. 

In  obtaining  these  pycnometer  weights,  it  is  unnecessary  to 
weigh  to  any  greater  degree  of  precision  than  the  nearest 
milligram. 


*Bock,  Jour.  Am.  Chem.  Soc.,  XLI,  359. 


XXIV.       STANDARDIZATION    OF    APPARATUS  183 

Calculate  the  density  of  the  test  solution  as  follows:  Divide 
the  apparent  weight  of  the  test  solution  by  the  apparent  weight  of 
the  water,  to  obtain  the  " apparent  specific  gravity."  Convert  the 
latter  to  "true  specific  gravity"  by  the  following  formula,  which 
gives  results  correct  within  four  units  in  the  fifth  decimal  place, 
equivalent  to  less  than  .01°  Brix. 

Let  D  =  true  sp.  gr. 

D'=  apparent  sp.  gr. 
Then  D  =  D'—  .001   (D'— 1) 

Tlx-n  find  the  equivalent  degree  Brix  from  the  20°/20°  column  in 
Table  1. 

EXAMPLE 

Weight  of  wrater  in  pycnometer  50.014  g 

Weight  of  test  solution  in  pycnometer  66.043  g 

J™11  =  1.32049 
50.014 

1.32049  —  .001  (1.32049  —  1)  -=  1.32049  —  .00032  =  1.32017 

From  the  table,  1.32017  sp.  gr.  at  20°  720°  C.  is  equivalent  to  65.25° 
Brix. 

Reading  of  Hydrometer:  Use  a  cylinder  provided  with  an 
overflow  as  shown  in  fig.  3,  p.  12,  Bureau  of  Standards  Circular 
16.  Provide  also  a  stirrer  consisting  of  a  glass  rod  slightly  longer 
than  the  cylinder  and  bent  into  a  spiral  at  the  bottom. 

Fill  the  cylinder  with  the  test  solution  at  a  temperature  of 
20°  C.  Immerse  the  hydrometer  carefully  slightly  beyond  (about 
y4  inch)  the  point  where  it  floats  naturally,  and  then  allow  it  to 
float  freely  until  it  has  assumed  the  temperature  of  the  liquid, 
the  hydrometer,  stir  the  liquid,  and  observe  the  temperature. 
If  this  is  not  exactly  20°,  bring  it  to  this  temperature,  then  im- 
merse the  hydrometer  as  before.  If  the  room  temperature  varies 
much  from  20°,  changes  in  temperature  may  be  avoided  by  keep- 
ing the  hydrometers  immersed  in  a  large  jar  of  water  at  20°  and 
transferring  them  immediately,  after  wiping,  to  the  cylinder  con- 
taining the  test  solution.  Make  all  readings  at  20°,  as  the  tempera- 
ture corrections  prescribed  for  sugar  solutions  will  not  be  the  same 
for  sulphuric  acid  solutions. 

To  eliminate  the  effect  on  the  reading  of  the  formation  of 
surface  films  of  impurities,  pour  into  the  funnel  sufficient  of  the 


184  METHOI>S  OP  ANALYSIS 

test  solution  (at  20°  C.)  to  cause  the  liquid  to  overflow  through 
the  spout.  Then  read  the  hydrometer.  Test  the  completeness  of 
the  surface  cleansing  by  repeating  the  operation;  the  readings 
will  approach  a  constant  value  as  the  surface  becomes  normal. 

Do  not  take  the  reading  until  the  liquid  and  hydrometer  are 
free  from  air  bubbles  and  at  rest.  When  the  reading  is  taken,  the 
hydrometer  must  not  be  in  contact  with  the  bottom  or  walls  of 
the  cylinder.  Read  the  scale  by  bringing  the  eye  upon  a  level 
with  the  surface  of  the  solution  so  that  the  latter  appears  as  a 
straight  line  and  not  an  ellipse,  and  note  where  the  border  line 
forming  the  bottom  of  the  meniscus  intersects  the  scale. 

The  reading  in  a  sulphuric  acid  solution  also  theoretically 
requires  a  correction  due  to  the  difference  in  surface  tension 
between  sulphuric  acid  and  sugar  solutions.  This  varies  with 
the  diameter  of  the  stem  of  the  hydrometer  and  the  density  of  the 
solution,  but  for  sugar  hydrometers  of  the  customary  sizes  and 
ranges  the  correction  is  so  small  that  it  may  be  disregarded. 

(c)  COMPARISON  METHOD 

Hydrometers  may  also  be  tested  by  comparison  with  standard 
hydrometers  certified  by  the  Bureau  of  Standards.  Use  a  cylinder 
large  enough  to  hold  the  standard  hydrometer  and  the  hydrometer 
to  be  tested  at  the  same  time,  and  employ  a  sulphuric  acid  solution 
at  room  temperature  as  the  liquid. 

Overflowing  to  remove  surface  contamination  is  unnecessary, 
since  the  effect  of  the  latter  on  two  hydrometers  of  similar  dimen- 
sions will  be  the  same. 

Immerse  and  read  the  hydrometers  otherwise  as  described 
before. 

Until  standard  hydrometers  are  several  years  old,  they  are 
liable  to  change  slightly  in  reading  as  the  result  of  seasoning. 
Standard  hydrometers  should  therefore  be  verified  at  least  once 
a  year  by  the  pycnometer  method  until  they  have  had  several 
years'  seasoning,  or  in  case  of  doubt  should  be  returned  to  the 
Bureau  of  Standards  for  re-test. 

(d)  BAUME  HYDROMETERS 

Verify  Baume  hydrometers,  for  testing  molasses,  in  a  similar 
manner  to  Brix  hydrometers.  Use  Table  1  for  obtaining  the 
density  in  degrees  Baume  from  the  specific  gravity  at  20°/20°  C. 
of  the  test  solution,  after  converting  the  apparent  specific  gravity 


XXIV.      STANDARDIZATION   OP   APPARATUS  185 

at  20°/20°  to  true  specific  gravity  at  20°/20°  by  the  formula 
previously  given.  This^  Baume  scale  is  based  on  a  modulus  of 
145  and  specific  gravity  at  20°/20°  C.  Check  the  enclosed  ther- 
mometer as  well  as  the  areometric  scale. 

4.     THERMOMETERS 

Verify  thermometers  by  comparison  with  suitable  standards. 
Use  water  for  temperatures  up  to  its  boiling  point,  and  oil  for 
higher  ranges. 

» 

5.     GRADUATION  MARKS 

The  following  methods  may  be  found  useful  for  making  the 
graduation  marks  distinct  on  thermometers  and  volumetric  glass- 
ware : 

(a)  Dip  in  a  solution  of  asphaltum,  wipe  off  the  excess  with 
a  smooth  piece  of  paper,  and  bake  at  a  temperature  sufficiently 
high  to  harden  the  asphaltum. 

(b)  Rub  with  a  soft  graphite  pencil. 

(c)  Fill   with    a   paste    made   by    mixing  lamp    black   and 
turpentine. 

(d)  Apply  a  mixture  of  oil  and  white  lead,  rub  softly  witli 
tissue  paper,  then  apply  dry,  powdered  zinc  oxide  and  again  rub 
gently  with  the  tissue  paper. 

6.     WEIGHTS 

Verify  weights  by  comparison  with  suitable  standards.  The 
present  standard  saccharimetric  normal  weight  is  26  grams.  Check 
normal  weights,  including  multiples  and  fractions,  and  counter- 
weighted  dishes  at  frequent  intervals. 

7.  POLARISCOPES  AND  POLARISCOPE  TUBES 

(a)     POLARISCOPES 

Verify  polariscopes  from  time  to  time  with  quartz  plates 
which  have  been  standardized  by  the  Bureau  of  Standards,  or 
have  been  carefully  compared  with  such  standard  plates.  Polari- 
scopes which  are  sent  to  the  Bureau  of  Standards  will  be  tested 
by  them  at  several  points  on  the  scale  and  a  certificate  of  correc- 
tions furnished. 


186  METHODS  OF  ANALYSIS 

See  Chap.  XXIII,  13  (b)  for  the  definition  of  the  100  degree 
point  of  the  saccharimetric  scale.  The  sugar  scale  now  employed 
by  the  Bureau  of  Standards  in  standardizing  saccharimeters  and 
quartz  plates  is  the  Bates-Jackson  scale,  which  differs  by  about 
0.1°  at  the  100°  point  from,  the  Herzfeld-Schonrock  scale,  the 
standard  formerly  in  use.  Pure  sugar  which  polarizes  100.0  on 
the  former  scale  will  polarize  100.1  on  the  latter. 

(b)     POLABISCOPE  TUBES 

Verify  the  length  of  polariscope  tubes  by  measurement.  Test 
for  eccentricity  of  mounting  of  the  caps  by  placing  the  tube,  with 
the  caps  on,  in  the  trough  of  a  polariscope  and,  while  revolving  it, 
viewing  the  opening  through  the  tube  with  reference  to  the  polari- 
scope field;  if  the  tube  has  been  properly  centered  and  the  caps 
are  free  from  eccentricity,  the  tube  opening  will  remain  in  the 
center  of  the  field  and  show  no  movement  during  rotation.  Test 
for  plane  parallelism  of  the  ends  of  the  tube  and  of  cover  glasses 
by  repeating  the  experiment  with  the  cover  glasses  in  position  and 
the  tube  filled  with  water ;  take  readings  also  at  different  positions 
during  rotation  to  make  sure  that  any  lack  of  plane  parallelism 
causes  no  optical  activity.  Test  metal  tubes,  which  may  become 
bent,  frequently  in  this  manner.  (See  Browne's  "Handbook  of 
Sugar  Analysis,"  pp.  154-5.) 

8.     REFRACTOMETERS 

Test  at  the  zero  point  with  distilled  water,  and  at  other  points 
with  standard  plates  or  solutions  made  up  by  weight  from  sugar 
of  accurately  determined  polarization. 

9.  CALORIMETERS 

Determine  the  water  equivalent  with  the  standard  heat  sam- 
ples of  the  Bureau  of  Standards  (benzoic  acid,  naphthalene,  and 
sugar).  All  thermometers  used  in  calorimetric  work  should  be 
certified  by  the  Bureau  of  Standards  and  the  necessary  corrections 
should  be  employed. 

10.  BIBLIOGRAPHY 

Refer  to  the  following  publications  of  the  Bureau  of 
Standards : 

Circular  3 — "Design  and  Test  of  Standards  of  Mass." 
Circular  8— "Testing  of  Thermometers." 


XXIV.       STANDARDIZATION   OF   APPARATUS  187 

Circular  9 — ''Testing  of  Glass  Volumetric  Apparatus. " 
Circular  11 — "Standardization  of  Bomb  Calorimeters." 
Circular  12 — "Verification  of  Polariscopic  Apparatus." 
Circular  16— "Testing  of  Hydrometers." 
Circular  19— "Standard  Density  and  Volumetric  Tables." 
Circular  25 — "Standard  Analyzed  Samples." 
Circular  44— " Polarimetry. " 

Miscellaneous — "Tables  of   Equivalents  of  the  U.   S.   Customary 
and  Metric  Weights  and  Measures." 


XXV.     REAGENTS 

This  chapter  covers  the  preparation  and  standardization  of 
reagents  which  have  a  general  application.  Reagents  used  for 
special  determinations  will  be  found  described  in  connection  with 
the  particular  determinations. 

1.     ACETIC  ACID,  DILUTE,  FOR  LIME  CAKE  ANALYSIS 
Mix  15  ml  of  the  99%  acetic  acid  with  1  liter  of  water. 

2.     ACETIC  ACID,  DILUTE,  FOR  SACCHARATE  CAKE 

ANALYSIS 

Dilute  1  part  of  the  99%  acetic  acid  with  4  parts  of  water. 

3.     ALPHA-NAPHTHOL 

Dissolve  5  grams  of  alpha-naphthol  in  100  ml  of  95%  alcohol. 
This  solution  should  give  the  reactions  described  in  Chap.  I,  13. 
If  the  sensibility  of  the  alpha-naphthol  is  poor,  the  strength  of 
the  solution  may  be  increased  to  10  or  20%,  if  necessary.  As  this 
solution  does  not  keep  well,  and  is  liable  to  become  contaminated, 
it  should  be  made  .up  in  small  quantities. 

4.     ALUMINA   CREAM 

(a)  Method  I:    Add  a  slight  excess  of  ammonium  hydroxide 
to  a  cold  saturated  solution  of  alum;  then  bring  to  a  faint  acid 
reaction  with  a  portion  of  the  original  alum  solution  retained  for 
the  purpose. 

(b)  Method  II:     A  preparation  free  from  dissolved  salts  is 
obtained  as  follows.     Add  a  slight  excess  of  ammonium  hydroxide 
to  a  cold  saturated  solution  of  alum,  allow  the  precipitate  to  settle 
and  wash  by  decantation  with  water  until  the  wash  water  gives 


XXV.      REAGENTS  189 

only  a  faint  reaction  for  sulphates  with  barium  chloride  solution. 
Pour  off   the   excess  of   water  until   the   cream   has  the   proper 

consistency. 

5.     AMMONIUM  CARBONATE 

Dissolve  1  part  of  the  crystallized  salt  in  a  mixture  of  3  parts 
of  water  and  1  part  of  ammonium  hydroxide. 

6.     AMMONIUM  OXALATE 

Dissolve  1  part  of  the  crystallized  salt  in  24  parts  of  water. 

7.     BARIUM  CHLORIDE,  GENERAL  REAGENT 
Dissolve  1  part  of  the  crystallized  salt  in  10  parts  of  water. 

8.     BARIUM    CHLORIDE    SOLUTION,    FOR   STANDARDIZ- 
ING SOAP  SOLUTION 

Dissolve  4.3574  grams  of  the  C.  P.  crystallized  salt 
(BaCl2.2H2O)  in  water  and  make  up  to  1  liter.  This  solution 
Ins  a  value  of  1  ml  =  .001  g  *CaO.  In  case  of  doubt  as  to  the 
purity  of  the  barium  chloride,  the  value  may  be  accurately  de- 
termined by  precipitating  with  an  excess  of  dilute  sulphuric  acid 
«i  ud  weighing  the  barium  sulphate.  Before  finishing  the  ignition 
add  a  few  drops  of  sulphuric  acid  so  that  any  barium  present  as 
<;  -rinded  barium  chloride  will  be  converted  to  sulphate. 

9.     FEHLING'S  SOLUTION 

Fehling's  Solution  (Soxhlet's  Modification)  consists  of  the 
following  two  solutions  which  are  mixed  in  equal  volumes  immedi- 
ately before  use. 

(a)  Copper  Sulphate   Solution:      Dissolve  34.639   grams  of 
C.  P.  crystallized  copper  sulphate  in  water,  and  dilute  to  a  volume 
of  500  ml. 

(b)  Alkaline  Tartrate  Solution:    Dissolve  173  grams  of  C.  P. 
vodium  potassium  tartrate  (Rochelle  salt)  and  50  grams  of  sodium 
hydroxide  in  water,  and  dilute  to  a  volume  of  500  ml.     Do  not 
n-e  the  commercial  grade  of  Rochelle  salt. 


190  METHODS  OP  ANALYSIS 

10.     HYDROCHLORIC  ACID  FOR  INVERSIONS 

Dilute  the  ordinary  C.  P.  acid  to  a  density  of  24.8—24.9° 
Brix  at  20°.  (1.1029  sp.  gr.  at  20°/4°  or  1.1049  sp.  gr.  at  20°  720°. ) 

11.     INDICATORS 

(a)  Cochineal:     Digest,  with  frequent  agitation,  3  grams  of 
pulverized  cochineal  in  a  mixture  of  50  ml  of  strong  alcohol  and 
200  ml  of  water  for  1  or  2  days  at  ordinary  temperature,  and  then 
filter. 

(b)  Methyl  Orcvnge:    Dissolve  1  part  of  the  dye  in  1000  parts 
of  water. 

(c)  Methyl  Red:    Dissolve  1  gram  of  methyl  red  (dimethyl- 
amino-azo-benzene-ortho-carbonic  acid)   in  100  ml  of  95%  alcohol. 

(d)  Phenolphthalein :  Dissolve  5  grams  of  the  powder  in 
500—600  ml  of  95%  ethyl  alcohol  or  refined  methyl  alcohol  (Colum- 
bian Spirit),  and  dilute  t<y  1  liter  with  water.  Denatured  alcohol 
or  commercial  "wood  alcohol"  must  not  be  used.  Then  add  a 
dilute  solution  of  sodium  hydroxide  until  a  faint  permanent  pink 
color  is  produced. 

12.     LEAD  ACETATE,  BASIC 

This  solution  is  the  clarifying  agent  commonly  used  in  the 
preparation  of  solutions  for  polarization.  Mix  together  1  part 
of  litharge,  3  parts  of  "sugar  of  lead,"  and  10  parts  of  water, 
using  commercial  chemicals  of  good  quality.  Boil  for  one-half 
hour  by  injecting  steam,  then  let  the  solution  cool  and  allow  the 
undissolved  material  to  settle.  Decant  the  clear  supernatant 
liquid  and  dilute  it  to  a  density  of  55°  Brix.  Preserve  the  solution 
in  wood,  glass,  or  earthenware  containers.  If  steam  is  not  avail- 
able, the  solution  may  be  prepared  by  using  hot  water  with  fre- 
quent stirring. 

13.     LEAD  ACETATE,  NEUTRAL 

This  solution  is  used  as  the  clarifying  agent  in  the  determina- 
tion of  *invert  sugar.  Make  up  a  concentrated  aqueous  solution 
of  "sugar  of  lead,"  neutralize  any  free  acid  or  alkali  with  sodium 
hydroxide  or  acetic  acid,  and  dilute  to  a  density  of  55°  Brix. 

*Chap.  I,  6. 


XXV.       REAGENTS  191 

14.     ORSAT  REAGENTS 

(a)  Potassium  Hydroxide  Solution:    To  be  used  for  the  ab- 
sorption of  carbon  dioxide   (C02).     Prepare  a  stock  solution  by 
adding  *330  grams  of  potassium  hydroxide  (not  purified  by  alco- 
hol) to  1  liter  of  water,  and  preserve  in  a  rubber-stoppered  bottle. 
One  filling  of  the  Orsat  pipette  will  make  about  150  carbon  dioxide 
determinations  in  flue  gas. 

(b)  Alkaline  Pyrogallol  Solution:     To  be  used  for  the  ab- 
sorption of  oxygen  (0).     Dissolve  10  grams  of  pyrogallol  (pyro- 
gallic  acid)   in  25  ml  of  water.     Transfer  to  the  second  pipette 
of  the   Orsat,   and   add   potassium   hydroxide   solution,   prepared 
as  in   (a),  until  both  arms  of  the  pipette  are  a  little  more  than 
half  filled.    Attach  the  seal  immediately  and  mix  the  two  solutions 
in  the  pipette  by  circulating  gas  back  and  forth  between  the  Orsat 
burette  and  the  pipette.    Renew  the  solution  when  the  absorption 
of  oxygen  becomes  slow.    One  filling  of  the  pipette  will  make  about 
40  oxygen  determinations  in  flue  gas. 

(c)  Acid  Cuprous  Chloride  Solution:     To  be  used  for  the 
absorption  of  carbon  monoxide  (CO).     Cover  53  grams  of  cupric 
chloride    (CuCl2.2H20)    and  75   grams  of  copper  turnings  with 
300  ml  of  concentrated  hydrochloric  acid,  and  allow  to  stand  in 
a  stoppered  bottle,  with  occasional  shaking,  for  24  hours  or  1  mger, 
until  the  solution  has  become  colorless  or  nearly  so.     Then  dilute 
with  150  ml  of  water  and  preserve  in  a  tightly  stoppered  bottle 
in  contact  with  copper  turnings.     Avoid  exposure  of  the  solution 
to  the  air.     When  saturated  with  carbon  monoxide,  the  solution 
may  be  renewed  by  heating  to  60 — 70°   to  drive  off  the  carbon 
monoxide,  and  will  then  be  as  efficient  as  it  was  originally. 

15.     PLATINIC  CHLORIDE  SOLUTION 

The  solution  should  contain  1  gram  of  metallic  platinum,  or 
2.65  grams  of  chloroplatinic  acid  (H2PtCl6.6H20)  in  every  10  ml. 

16.     PLATINUM  RECOVERY 

Preserve   all  residues   from   potassium   determinations   which 
contain  platinum,  including  both  the  precipitated  potassium  pla- 


*Some  textbooks  recommend  a  stronger  solution,  viz.  500  grams  of 
potassium  hydroxide  dissolved  in  1  liter  of  water. 


192  METHODS  OP  ANALYSIS 

tinic  chloride  as  well  as  the  filtrates  and  washings  from  platinic 
chloride  precipitations.  Dissolve  the  potassium  platinic  chloride 
off  the  Gooch  mats  by  means  of  hot  water. 

Remove  the  alcohol  from  the  alcoholic  solutions  by  distillation, 
concentrate  the  solutions  in  a  large  porcelain  dish  on  a  water 
bath,  and  reduce  to  metallic  platinum  by  the  addition  of  hydro- 
chloric acid  and  C.  P.  zinc  or  aluminum,  heating  until  the  zinc  or 
aluminum  is  completely  dissolved.  Decant  the  supernatant  liquid 
and  wash  the  spongy  platinum  by  decantation  with  water.  Bring 
the  platinum  upon  a  filter  and  wash  till  the  filtrate  shows  no  acid 
reaction.  Ignite  the  filter  containing  the  platinum  sponge  in  a 
platinum  or  porcelain  crucible  and  weigh.  Transfer  the  platinum 
sponge  to  a  porcelain  dish,  add  about  four  times  its  weight  of 
concentrated  hydrochloric  acid  heat  on  a  water  bath,  and  add 
concentrated  nitric  acid  in  small  portions  until  the  platinum  is 
completely  dissolved.  Evaporate  two  or  three  times  with  hydro- 
chloric acid  to  expel  the  nitric  acid,  then  evaporate  to  a  syrupy 
consistence,  take  up  with{  water,  and  filter.  Dilute  the  filtrate  to 
the  volume  which  will  yield  a  platinum  solution  of  the  standard 
strength,  viz.,  1  gram  in  10  ml. 

It  is  important  to  use  zinc  or  aluminum  of  high  purity  (com- 
mercial grades  are  not  suitable)  and  to  make  sure,  by  testing  the 
filtrate  with  more  zinc  or  aluminum,  that  the  platinum  has  been 
completely  precipitated. 

17.     SEA  SAND 

For  moisture  determinations  use  clean  sea  sand,  free  from 
any  great  amount  of  dust.  Screen  it  through  a  40  mesh  sieve 
and  discard  the  portion  retained  by  the  sieve.  Digest  the  remain- 
der with  hot,  commercial  hydrochloric  acid,  and  wash  the  sand 
thoroughly  in  a  current  of  water,  then  decant  the  excess  of 
water,  and  dry  on  a  hot  plate. 

The  dried  residues  from  moisture  determinations  may  con- 
veniently be  loosened  by  soaking  in  water  and  then  transferred 
to  a  jar,  or  suitable  container.  After  washing  the  sand  in  a  cur- 
rent of  water  and  drying,  as  before,  it  may  then  be  used  again 
for  the  same  purpose. 

18.     SODIUM  CARBONATE 

Dissolve  1  part  of  the  anhydrous  salt,  or  2.7  parts  of  the 
crystals  (Na2C03.10H20)  in  5  parts  of  water. 


XXV.      REAGENTS  193 

19.     SODIUM  AMMONIUM  PHOSPHATE. 

Dissolve  1  part  of  the  crystals  (microcosmic  salt)  in  17  parts 
of  water. 


20.     SODIUM  HYDROGEN  PHOSPHATE 

Dissolve  1  part  of  the  crystals  of  disodium  hydrogen  phos- 
phate in  10  parts  of  water. 


21.     STANDARD  ACID  AND  ALKALI   SOLUTIONS 

(a)     PRIMARY  STANDARDS 

A  standard  sodium  carbonate  solution  will  probably  prove 
the  most  serviceable  for  general  use.  In  case  of  doubt  as  to  the 
purity  of  the  sodium  carbonate,  or  as  an  additional  check,  verify 
the  strength  of  the  finally  prepared  solution  by  one  of  the  other 
methods  given. 

(1)  Sodium  Carbonate:     Ignite  sodium  carbonate  or  bicar- 
bonate of  the  *highest  purity  obtainable  to  constant  weight  in  a 
t  platinum  dish  or  crucible  at  a  dull  red  heat,  being  careful  not 
to  allow  any  of  the  material  to  fuse.     From  the  freshly  ignited 
material,   cooled   and  kept  in   a  desiccator   over  sulphuric   acid, 
standard  solutions  may  be  made  up  in  accordance  with  the  table 
given  below.     1.8906  parts  of  Na2C03  are  equivalent  to  1  part  of 
CaO.    In  titrating,  use  methyl  orange  as  indicator. 

Strength  of  Grams  of  Na2C03 

Solution  per  Liter 

Normal    53.0025 

1  ml  =  .05     g  CaO    94.5292 

1  ml  =  .001  g  CaO    1.8906 

(2)  Benzoin  Acid:     A  sodium  hydroxide  solution   may  be 
standardized  by  titrating  against  weighed  amounts  of  benzoic  acid 
of  the  Bureau  of  Standards.     A  sulphuric  acid  solution  is  then 
standardized  against  the  sodium  hydroxide  solution.     Prepare  the 
linizoic  acid  by  heating  in  a  covered  platinum  dish  in  an  oven  to 
about  130°   (not  over  140°).     As  soon  as  fusion  is  complete,  pour 


*Use  the  grade  "C.  P.  Special  for  Standardizing"  and  not  the  ordinary 
"C.  P." 

IA  convenient  arrangement  for  igniting  sodium  carbonate  is  shown 
in  \V.  W.  Scott's  "Standard  Methods  of  Chemical  Analysis,"  p.  501. 


194  METHODS  OF  ANALYSIS 

it  into  a  test  tube  or  into  glass  tubes  sealed  at  one  end  which  have 
been  thoroughly  cleaned  and  dried.  After  the  material  has  solidi- 
fied, break  away  the  glass  and  preserve  the  sticks  in  a  glass- 
stoppered  bottle.  The  material  is  not  hygroscopic  except  after 
long  standing.  Dissolve  the  benzoic  acid  in  95%  alcohol  (20  ml 
for  a  1  gram  sample)  and  make  a  blank  test  on  the  same  volume 
of  alcohol,  applying  any  correction  thus  found  necessary.  Use 
phenolphthalein  as  indicator.  4.3547  parts  of  pure  benzoic  acid 
(CCH5C02H)  are  equivalent  to  1  part  of  CaO. 

(3)  Gravimetric  Method:  The  strength  of  a  sulphuric  acid 
solution  may  be  determined  by  diluting  with  water,  precipitating 
with  barium  chloride,  and  weighing  as  barium  sulphate  in  the 
regular  manner.  Sulphates,  if  present,  will  vitiate  the  result, 
but  should  not  be  present  in  any  ordinary  C.  P.  sulphuric  acid. 
Serious  error  will  be  caused  if  any  marked  excess  of  barium 
chloride  is  used,  owing  to  the  occlusion  of  barium  chloride  in  the 
precipitate;  the  best  plan  is  perhaps  to  determine  the  theoretical 
amount  of  barium  chloride  needed  and  to  add  about  2  or  3%  more 
than  this  amount.  After  weighing  the  ignited  barium  sulphate, 
add  a  drop  or  two  of  sulphuric  acid,  evaporate  the  acid  on  a 
radiator,  and  reignite  and  reweigh  to  determine  if  any  reduced 
barium  sulphide  was  present  after  the  first  ignition.  As  the 
barium  sulphate  precipitations  must  stand  over  night,  this  method 
is  slow  for  adjusting  a  sulphuric  acid  solution  to  a  definite  strength, 
and  is  chiefly  useful  for  standardizing  a  solution  which  is  not  made 
up  to  a  definite  strength,  or  for  verifying  the  value  of  a  solution 
already  standardized  by  another  method. 

(b)     N/28  SULPHURIC  ACID 

As  large  quantities  of  this  acid  (1  ml  =  .001  g  CaO )  are 
required,  it  should  be  made  up  in  carboys  or  large  bottles  of  about 
40  liters  capacity.  Prepare  a  solution  slightly  over  strength  by 
slowly  pouring  *75  grams  (40.8  ml)  of  sulphuric  acid  of  1.84 
sp.  gr.  into  40  liters  of  water  in  a  carboy,  and  mix  thoroughly  by 
a  current  of  air. 

Prepare  a  standard  sodium  carbonate  solution  (1  ml  =  .001  g 
CaO)  as  in  "(a),  (1),"  by  dissolving  1.8906  grams  of  freshly 
ignited  sodium  carbonate  in  neutral  water  and  making  up  to  1 


*It  may  be  more  convenient  to  make  up  first  an  approximately  normal 
solution  and  then  dilute  this  in  the  proportion  of  1  part  of  the  normal 
solution  to  27  parts  of  water.     Then  titrate  the  diluted  solution  in  the 
manner  described. 


XXV.      REAGENTS  195 

liter.  Titrate  25 — 50  ml  of  the  standard  sodium  carbonate  solution 
to  neutrality  with  the  sulphuric  acid  solution,  adding  several 
drops  of  methyl  orange  as  indicator.  Calculate  the  additional 
amount  of  water  which  must  be  added,  as  in  the  following  example : 

If  40  ml  of  the  sodium  carbonate  requires  39.2  ml  of  the  acid,  then 

40 

-  1  =  .0204  ml  of  water  to  be  added  per  ml  of  original  solu- 

ou.6 

tion,  or,  to  the  original  volume  of  40,000  ml,  .0204  X  40,000  =  816 
ml  of  water  must  be  added.  Add  this  amount  of  water,  mix  well 
with  air,  and  titrate  again.  Repeat  the  above  procedure,  viz., 
dilution  and  titration,  until  the  strength  of  the  acid  is  exactly 
equal  to  that  of  the  sodium  carbonate.  As  a  check  against  possible 
error  in  weighing  or  in  volumetric  apparatus,  the  final  solution 
may  then  be  titrated  against  a  suitable  weighed  amount  of  the 
ignited  sodium  carbonate. 

(c)  N/28  SODIUM  HYDROXIDE 

As  N/28  sodium  hydroxide  is  not  required  in  large  quantities, 
and  is  unstable  due  to  absorption  of  carbon  dioxide  from  the  air 
and  its  solvent  action  on  glass,  it  is  best  to  prepare  this  solution  in 
small  amounts  and  check  it  frequently  against  the  N/28  sulphuric 
acid.  Use  about  *1.6  grams  of  sodium  hydroxide  per  liter  of 
water.  Titrate  against  the  N/28  acid  and  dilute  with  water,  etc., 
until  its  strength  is  exactly  equal  to  that  of  the  standard  acid. 

(d)  STEPFEN  NITRIC  ACID  (1  ml  =  .05  g  CaO) 

As  large  quantities  of  this  acid  are  required,  it  should  be  made 
up  in  carboys.  Make  up  170  grams  (120  ml)  of  nitric  acid  of 
1.42  sp.  gr.  to  1  liter,  or  mix  6800  grams  (4800  ml)  of  the  acid  with 
35200  ml  of  water.  After  mixing,  titrate  against  a  sodium  car- 
bonate solution  (1  ml  =  .05  g  CaO)  made  by  dissolving  23.632 
grams  of  freshly  ignited  sodium  carbonate,  prepared  as  in  "(a), 
(1),"  in  water  and  making  up  to  a  volume  of  250  ml.  Adjust 
the  acid  to  the  proper  strength  by  titration  and  dilution  as  de- 
scribed under  (b). 

(e)  STEFFEN  SODIUM  HYDROXIDE  (1  ml  =  .05  g  CaO) 

Large  amounts  of  this  solution  are  required,  but  it  should  not 
be  made  up  in  carboy  lots  owing  to  its  liability  to  change  in 
strength.  Dissolve  about  80  grams  of  sodium  hydroxide  in  1  liter 
of  water  and  standardize  against  the  Steffen  nitric  acid.  If  de- 
sired, a  solution  slightly  over  strength  may  be  made  up  in  carboy 


*See  footnote  on  previous  page. 


196  METHODS  OF  ANALYSIS 

lots  to  serve  as  the  source  of  supply  for  the  preparation  of  smaller 
quantities  of  the  standard  solution. 

22.     STANDARD  SOAP  SOLUTION 

As  soap  solution  is  subject  to  some  alteration  in  strength  on 
long  standing,  the  standard  solution  should  be  made  up  in  quan- 
tities which  will  last  for  not  more  than  3  or  4  weeks,  or  should  be 
restandardized  at  the  end  of  this  time. 

(a)  PREPARATION 

(1)  Method  I:    Dissolve  20  grams  of  pure  potassium  hydrox- 
ide in  25  ml  of  water  and  add  200  ml  of  95%  ethyl  alcohol.    Add 
100  ml  of  best,  genuine  olive  oil  and  heat  on  a  water  bath  in  a 
flask  provided  with  a  reflux  condenser  until  saponification  is  com- 
plete,   recognizable   by  the   fact  that  several   drops   of   the   clear 
solution,  when  mixed  with  water,  cause  no  turbidity.     Pour  the 
solution  into  3  liters  of  water,  mix  well,  and  add  a  calcium  chloride 
solution  as  long  as  a  precipitate  is  formed.    Filter  off  the  precipi- 
tate through  a  fine  cloth,  and  press  to  remove  the  mother  liquor 
as  completely  as  possible.     Mix  the  precipitate   intimately   with 
40%  of  its  weight  of  potassium  carbonate  in  a  large  mortar,  and 
extract  with  several  portions  of  95%  ethyl  alcohol,  using  a  water 
bath  and  reflux  condenser  as  before.     Mix  the  various  portions, 
filter,  and  preserve  in  a  stoppered  bottle.    Use  this  strong  solution 
of  potassium  soap  as  a  source  of  supply  for  the  preparation  of 
the  standard  solution,  which  is  made  by  diluting  to  the  approxi- 
mate strength  with  60%   alcohol  and-  standardizing  as  described 
below. 

(2)  Method  II:    Dissolve  sodium  oleate,  or  shavings  of  the 
best  Castile  soap  obtainable,  in  60%  alcohol. 

(b)  STANDARDIZATION 

Prepare  a  barium  chloride  solution,  as  described  in  "8," 
containing  4.3*574  grams  of  the  C.  P.  crystallized  salt  (BaCl,.2H.,0) 
in  1  liter,  using  the  same  kind  of  water  which  is  employed  for 
dilution  in  the  standardization  test  described  below.  Transfer 
10  ml  with  a  pipette  to  an  8  oz.  glass  bottle  provided  with  a 
ground  stopper  and  marked  at  the  point  at  which  it  holds  50  ml, 
and  fill  to  the  50  ml  mark  with  water.  Add  a  drop  of  phenolph- 
thalein  and  then  add  N/28  sodium  hydroxide  a  drop  at  a  time 


XXV.       REAGENTS  197 

until  a  permanent  pink  color  is  produced;  unless  the  water  is  of 
very  poor  quality  one  drop  should  be  sufficient.  Then  add  the 
soap  solution  in  small  quantities  from  a  burette;  after  each  addi- 
tion, stopper  the  bottle  and  shake  vigorously.  Take  as  the  end 
point  the  *formation  of  a  fine  foam  5  mm  in  depth  which  will  last 
five  minutes.  Make  a  blank  test  on  50  ml  of  the  water  used  for 
dilution,  adding  a  drop  of  phenolphthalein  and  then  N/28  sodium 
hydroxide  a  drop  at  a  time  until  a  permanent  pink  color  is  pro- 
duced. Subtract  from  the  number  of  milliliters  of  soap  solution 
used  in  the  standardization  test  the  number  of  milliliters  of  soap 
solution  required  by  50  ml  of  the  water  in  the  blank  test. 

Calculate  from  the  above  the  t  dilution  necessary  to  reduce  the 
solution  to  such  a  strength  that  it  is  exactly  equal  to  the  barium 
chloride  solution,  i.  e.,  so  that  10  ml  of  the  barium  chloride  will 
be  exactly  neutralized  by  10  ml.  (corrected)  of  the  soap  solution. 
After  diluting,  ^standardize  and  continue  in  this  manner  until 
the  strength  is  accurately  adjusted. 

One  ml  of  the  standard  soap  solution  is  equivalent  to  .001 
gram  of  CaO. 

23.    WATER,  DISTILLED 

Distilled  water  produced  from  raw  water  of  poor  quality  in 
the  usual  laboratory  still  is  not  always  what  it  should  be.  One 
should  occasionally  test  the  reaction  by  titrating  a  measured 
amount  with  phenolphthalein  as  indicator,  and  determine  the 
amount  of  solids  present  by  evaporating  a  measured  amount  and 
drying  at  100 — 105° ;  from  these  data  one  can  determine  the  suita- 
bility of  the  water  for  the  purpose  in  question.  When  the  raw 
water  contains  large  amounts  of  bicarbonates,  the  distilled  water 
is  frequently  quite  acid  from  the  presence  of  dissolved  carbon 
dioxide  and  is  quite  unsuitable  for  acidimetric  titrations.  In  this 
case  boiling  the  water  after  distillation  until  the  carbon  dioxide 
is  all  expelled  will  generally  yield  a  water  of  neutral  reaction. 

24.     ZINC  NITRATE   SOLUTION 

This  solution  is  used  to  decompose  calcium  saccharate  in  the 
analysis  of  lime  cake.  Dissolve  1  part  of  commercial  zinc  nitrate 
in  10  parts  of  water. 


*See  Chap.  I,  12. 

tlf  a  =  no.  of  ml  of  the  soap  solution  required  by  10  ml  of  the  standard 
barium  chloride  solution,  and  x  =  volume  in  ml  to  which  each  liter  must 
be  diluted,  then  x  =  10000  -=-  a.  E.  g.,  if  a  =  9.25,  x  =  1081,  i.  e.,  81  ml 
of  water,  or  60%  alcohol,  must  be  added  to  each  1000  ml  of  the  original 
soap  solution. 


XXVI.     MISCELLANEOUS 

A  few  subjects  of  not  great  length  which  cannot  well  be 
classified  elsewhere  are  treated  in  this  chapter. 

1.     MOISTURE  TESTS  OF  SUGAR  IN  STORAGE 

* 

The  sugar  in  storage  in  the  warehouses  should  be  sampled 
and  analyzed  as  described  below  during  the  entire  intercampaign, 
or  up  to  the  time  when  all  sugar  has  been  shipped. 

SAMPLING 

Sample  on  the  15th  and  the  last  day  of  every  month ;  if  a 
sampling  day  falls  on  Sunday  or  a  holiday,  take  the  samples  on 
the  next  succeeding  working  day.  Take  the  first  set  of  samples 
on  the  first  sampling  day  after  the  sugar  end  has  finished,  pro- 
vided that  a  week  has  elapsed  since  that  time ;  if  the  elapsed  period 
is  less  than  a  week,  the  sampling  may  be  deferred  until  a  half- 
month  later. 

Take  separate  samples  from  the  outside  bag  at  3  points  of  each 
location,  as  follows: 

(a)  At  a  point  3  tiers  from  the  top  of  the  pile. 

(b)  At  the  middle  of  the  pile. 

(c)  At  a  point  3  tiers  from  the  bottom  of  the  pile. 

The  selection  of  the  locations  for  sampling  is  largely  gov- 
erned by  the  accessibility.  The  aisles  and  cross  passages  will 
usually  afford  opportunity  to  distribute  the  sampling  locations 
suitably  throughout  the  warehouses.  It  is  desirable  to  draw  a 
diagram,  keeping  this  for  reference  and  furnishing  a  copy  with 
the  first  report. 

Sample  one  bag  only  at  each  point,  and  mark  this  bag  in 
order  that  the  same  bag  may  be  sampled  throughout  the  storage 


XXVI.      MISCELLANEOUS  199 

period.  There  should  be  one  location  (3  samples)  for  at  least  every 
25,000  bags  in  storage,  and  at  least  five  locations  in  every  ware- 
house. Continue  the  sampling  at  every  location  until  the  sugar 
at  the  location  has  been  shipped.  In  addition  take  samples  at  the 
point  of  shipment  of  "Standard,"  "Table"  sugar,  etc. 

Take  all  samples  with  a  small  trier  from  the  interior  of  the 
bag,  avoiding  the  sugar  immediatly  next  to  the  sack.  Use  1x3 
in.  rubber  stoppered  test  tubes  as  containers.  Before  use,  clean 
them  carefully,  heat  them  in  a  drying  oven  together  with  the 
stoppers,  and  cool  in  a  desiccator. 
ANALYSIS 

Allow  the  samples  to"  stand  in  the  containers  long  enough  so 
that  the  sugar  will  attain  the  temperature  of  the  laboratory,  then 
weigh  out  10  grams  in  each  case  and  determine  the  moisture  as  in 
Chap.  II,  23. 

2.  SODA  ASH  AND  CAUSTIC  SODA 

Sample  each  carload  or  lot  received  and  analyze  according  to 
the  methods  of  the  Solvay  Process  Company  (Technical  Bulletins 
Nos.  1  and  2). 

3.  MURIATIC  ACID 

If  the  acid  is  received  in  tank  cars,  sample  each  carload  lot. 
If  it  is  received  in  carboys,  sample  a  number  of  carboys  and  test 
the  individual  samples  to  determine  if  there  is  any  variation,  also 
calculate  the  average  of  the  individual  tests. 

Determine  the  density  in  degrees  Baume.  Muriatic  acid  is 
usually  sold  on  a  specification  of  18°  Be.  The  scale  employed  is 
the  *American  Baume  scale,  which  is  based  on  a  modulus  of  145 
and  sp.  gr.  at  60°/60°  F.  The  determination  may  be  made  at 
20°  C.  with  a  Brix  hydrometer  and  the  reading  tranposed  directly 
to  degrees  Baume  by  the  use  of  Table  1  without  appreciable  error. 

4.  BARIUM  OXIDE 

Sample  each  lot  of  barium  oxide  received.  Grind  rapidly, 
protecting  the  material  from  exposure  to  the  air  as  it  absorbs 
carbon  dioxide  rapidly. 

Determine  the  total  water-soluble  barium  as  follows:  Weigh 
out  3 — 4  grams,  transfer  to  a  200  ml  volumetric  flask,  add  at  least 


*Bureau  of  Standards,  Circ.  19,  5th  ed.,  pp  34-36. 


200  METHODS  OF  ANALYSIS 

150  ml  of  distilled  water  free  from  carbon  dioxide,  and  boil  until 
all  soluble  matter  has  been  dissolved.  Cool,  make  up  to  the  mark, 
and  filter  through  a  dry  filter,  keeping  the  funnel  covered  to  pre- 
vent absorption  of  carbon  dioxide  from  the  air.  Transfer  50  ml 
of  the  filtrate  to  a  beaker,  dilute  to  a  volume  of  about  200  ml,  make 
slightly  acid  with  hydrochloric  acid,  and  precipitate  with  hot 
dilute  sulphuric  acid  in  the  regular  manner,  proceeding  as  in 
Chap.  XIII,  8.  Multiply  the  weight  of  BaS04  by  .6570  to  obtain 
the  BaO  equivalent  of  the  water-soluble  barium  present. 

The  weights  and  volumes  prescribed  above  must  be  adhered 
to,  in  order  that  the  limit  of  solubility  of  barium  hydroxide  may 
not  be  exceeded. 


5.     INSECTICIDES 

The  determination  of  total  and  water-soluble  arsenic  in  Paris 
Green  and  other  arsenicals  should  be  made  according  to  the 
"Methods  of  Analysis  of  the  Association  of  Official  Agricultural 
Chemists." 


6.     MISCELLANEOUS  SUPPLIES 

No  methods  are  given  or  prescribed  in  this  book  for  other  mis- 
cellaneous supplies  such  as  lubricating  oils,  paints,  rubber  goods, 
etc.,  because  chemical  analyses  in  such  cases  are  mostly  only  of 
value  when  correlated  with  service  tests.  Methods  may  be  found 
in  the  standard  textbooks,  among  which  may  be  particularly 
mentioned  "Some  Technical  Methods  of  Testing  Miscellaneous 
Supplies,"  by  Percy  H.  Walker,  a  miscellaneous  publication  of 
the  Bureau  of  Standards. 


XXVII.      TABLES 


201 


TABLE  1 
BRIX,  BAUME,  AND  SPECIFIC  GRAVITY  OF  SUGAR  SOLUTIONS 

Table  showing  equivalent  degrees  Brix,  degrees  Baume,  specific  gravity  at  20°  720°  C.,  pounds 
r  cubic  foot,  and  pounds  of  dry  substance  per  cubic  foot,  from  *values  of  the  U.  S.  Bureau  of 


pe 

Standards. 


Explanation 

The  Baume  scale  is  based  on  a  modulus  of  145  and  is  derived  from  specific  gravities  at 
20°/20°C.  (Bureau  of  Standards  Baume  scale  for  sugar  solutions.)     That  is,  if  d=  degrees  Baume 
and  s=specific  gravity  at  20°/20°C., 

Then  d=  145-  145/s 

The  values  for  fspecific  gravity  at  20°/20°C.  represent  true  specific  gravity,  i.  e.  the  ratio  of 
the  weights  in  vacua  of  equal  volumes  of  the  sugar  solution  and  of  water,  based  on  the  deter- 
minations of  Plato. 

The  values  for  "pounds  per  cubic  foot"  represent  weights  at  20°C.  in  air  against  brass  weights. 

The  values  for  "pounds  of  dry  substance  per  cubic  foot"  are  calculated  by  multiplying  the 
"pounds  per  cubic  foot"  by  the  percentage  of  dry  substance  represented  by  the  "degrees  Brix." 
For  impure  sugar  solutions  these  values  are  only  approximate. 


Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 

Cubic 
Foot 

Pounds 
Dry  Sub 
per 
Cu.  Ft. 

Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 

Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

0.0 

0.00 

1.00000 

62.25 

0.00 

2.0 

1.12 

1.00779 

62.73 

1.25 

0.1 

0.06 

1.00039 

62.27 

0.06 

2.1 

1.18 

1.00818 

62.76 

1.32 

0.2 

0.11 

1.00078 

62.30 

0.12 

2.2 

1.23 

1.00858 

62.78 

1.38 

0.3 

0.17 

1.00117 

62.32 

0.19 

2.3 

1.29 

1.00897 

62.81 

1.45 

0.4 

0.22 

1.00155 

62.35 

0.25 

2.4 

1.34 

1.00P36 

62.83 

1.51 

0.5 

0.28 

1.00194 

62.37 

0.31 

2.5 

1.40 

1.00976 

62.86 

1.57 

06 

0.34 

1.00233 

62.40 

0.37 

2.6 

1.46 

1.01015 

62.88 

1.64 

0.7 

0.39 

1.00272 

62.42 

0.44 

2.7 

1.51 

1.01054 

62.91 

1.70 

0.8 

0.45 

1.00311 

62.44 

0.50 

2.8 

1.57 

1.01093 

62.93 

1.76 

0.9 

0.51 

1.00350 

62.47 

0.56 

2.9 

1.62 

1.01133 

62.96 

1.83 

.0 

0.56 

1.00389 

62.49 

0.62 

3.0 

.68 

1.01172 

62.98 

1.89 

1 

0.62 

1.00428 

62.52 

0.69 

3.1 

.74 

1.01211 

63.00 

1.96 

2 

0.67 

1.00467 

62.54 

0.75 

3.2 

.79 

1.01251 

63.03 

2.02 

3 

0.73 

1.00506 

62.56 

0.81 

3.3 

.85 

1.01290 

63.05 

2.08 

.4 

0.79 

1.00545 

62.59 

0.88 

3.4 

.90 

1.01330 

63.08 

2.14 

.5 

0.84 

1.00584 

62.61 

0.94 

3.5 

1.96 

1.01369 

63.10 

2.21 

.6 

0.90 

1.00623 

62.64 

1.00 

3.6 

2.02 

1.01409 

63.13 

2.27 

.7 

0.95 

1.00662 

62.66 

1.07 

3.7 

2.07 

1.01448 

63.16 

2.34 

.8 

1.01 

1.00701 

62.69 

1.13 

3.8 

2.13 

1.01488 

63.18 

2.40 

.9 

1.07 

1.00740 

62.71 

1.19 

3.9 

2.18 

1.01528 

63.20 

2.46 

*Circulars  19  and  44. 

fThe  volume  in  milliliters,  of  a  given  weight  of  liquid  in  grams  in  air,  is  obtained  from  the  table  as  follows-  Let 
D  =  true  sp.  gr.  at  20°/20°  as  given  in  the  table,  D'  =  apparent  sp  gr.  at  20°/20°  (ratio  of  weights  in  air),  W  =  weight 
in  grams  of  liquid  in  air,  and  V  =  volume  of  liquid  at  20°  in  milliliters. 

Then  D7  =  D  +  .001  (D— 1) 
AndV  =  W  -=-  .99720' 
Conversely,  to  find  W  if  V  is  known 

W  =  .  9972  V  IX 

The  constant  .  9972  is  the  weight  in  grams  of  1  ml  of  water  at  20°  in  air.  The  formula  for  D'  gives  results  which 
are  accurate  within  four  units  in  the  fifth  decimal  place.  See  Chapter  XXIV,  3,  for  instructions  for  use  of  the  table 
in  standardizing  hydrometers. 


202 


METHODS  OP  ANALYSIS 


TABLE  1— Continued 


Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 

Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

4.0 

2.24 

.01567 

63.23 

2.53 

8.0 

4.46 

1.03176 

64.23 

5.14 

4.1 

2.29 

.01607 

63.25 

2.59 

8.1 

4.52 

1.03217 

64.25 

5.20 

4.2 

2.35 

.01647 

63.28 

2.66 

8.2 

4.58 

1.03258 

64.28 

5.27 

4.3 

2.40 

.01687 

63.30 

2.72 

8.3 

4.63 

1.03299 

64.30 

5.33 

4.4 

2.46 

.01726 

63.33 

2.79 

8.4 

4.69 

1.03340 

64.33 

5.40 

4.5 

2.52 

.01766 

63.36 

2.85 

8.5 

4.74 

1.03381 

64.36 

5.47 

4.6 

2.57 

.01806 

63.38 

2.92 

8.6 

4.80 

1.03422 

64.38 

5.54 

4.7 

2.63 

.01846 

63.40 

2.98 

8.7 

4.85 

1.03463 

64  .  40 

5.60 

4.8 

2.68 

.01886 

63.43 

3  04 

8.8 

4.91 

1.03504 

64.43 

5.67 

4.9 

2.74 

.01926 

63.45 

3.11 

8.9 

4.96 

1.03545 

64.46 

5.74 

5.0 

2.79 

1.01965 

63.47 

3.17 

9.0 

5.02 

.03586 

64.48 

5.80 

5.1 

2.85 

1.02005 

63.50 

3.24 

9.1 

5.07 

.03627 

64.50 

5.87 

5.2 

2.91 

1.02045 

63.52 

3.^0 

9.2 

5  13 

.03668 

64.53 

5.94 

5.3 

2.96 

1.02085 

63.55 

3.37 

9.3 

5.19 

.03709 

64.56 

6.00 

5.4 

3.02 

1.02125 

63.57 

3.43 

9.4 

5.24 

.03750 

64.58 

6.07 

5.5 

3.07 

1.02165 

63.60 

3.50 

9.5 

5.30 

1.03792 

64.61 

6.14 

5.6 

3.13 

1.02206 

63.62 

3  56 

9.6 

5.35 

1.03833 

64.63 

6.20 

5.7 

3.18 

1.02246 

63.65 

3  63 

9.7 

5.41 

1.03874 

64.66 

6.27 

5.8 

3.24 

1.02286 

63.67 

3.69 

9.8 

5.46 

1.03915 

64.69 

6.34 

5.9 

3.30 

1.02321 

63.70 

3.76 

9.9 

5.52 

1.03957 

64.72 

6.41 

6.0 

3.35 

1.02366 

63.72 

3.82 

10.0 

5.57 

1.03998 

64.74 

6.47 

6.1 

3.41 

1.02407 

63.75 

3.89 

10.1 

5.63 

1.0i039 

64.77 

6.54 

6.2 

3.46 

1.02447 

63.77 

3.95 

10.2 

5.68 

1.04081 

64.79 

6.61 

6.3 

3.52 

1.02487 

63.80 

4.02 

10.3 

5.74 

1.04122 

64.82 

6.68 

6.4 

3.57 

1.02527 

63.82 

4.08 

10.4 

5.80 

1.04164 

64.84 

6.74 

6.5 

3.63 

1.02568 

63.85 

4.15 

10.5 

5.85 

1.04205 

64.87 

6.81 

6.6 

3.69 

1.02608 

63.87 

4.21 

10.6 

5.91 

1.04247 

64.90 

6.88 

6.7 

3.74 

1.02648 

63.90 

4.28 

10.7 

5.96 

1.04288 

64.92 

6.95 

6.8 

3.80 

1.02689 

63.92 

4.34 

10.8 

6.02 

.04330 

64.95 

7.01 

6.9 

3.85 

1.02729 

63.95 

4.41 

10.9 

6.07 

.04371 

64.97 

7.08 

7.0 

3.91 

1.02770 

63.97 

4.47 

11.0 

6.13 

.04413 

65.00 

7.15 

7.1 

3.96 

.02810 

64.00 

4.54 

11.1 

6.18 

.04455 

65.03 

7.22 

7.2 

4.02 

.02851 

64.03 

4.60 

11.2 

6.24 

.04497 

65.05 

7.29 

7.3 

4.08 

.02892 

64.05 

4.67 

11.3 

6.30 

.04538 

65.08 

7.35 

7.4 

4.13 

.02932 

64.08 

4.74 

11.4 

6.35 

1.04580 

65.11 

7.42 

7.5 

4.19 

.02973 

64.10 

4.80 

11.5 

6.41 

1.04622 

65.13 

7.49 

7.6 

4.24 

.03013 

64.13 

4.87 

11.6 

6.46 

1.04664 

65.16 

7.56 

7.7 

4.30 

.03054 

64.15 

4.94 

11.7 

6.52 

1.04706 

65.18 

7.63 

7.8 

4.35 

.03095 

64.18 

5.01 

11.8 

6.57 

1.04747 

65.21 

7.69 

7.9 

4.41 

.03136 

64.20 

5.07 

11.9 

6.63 

1  .  04789 

65.23 

7.76 

XXVII.      TABLES 


203 


TABLE  1— Continued 


Degrees 

Hrix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
0°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

Degrees 
Brix  or 

%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

12.0 

6.68 

1.04831 

65.26 

7.83 

16.0 

8.89 

1.06534 

66.32 

10.61 

12  1 

6.74 

1.04873 

65.29 

7.90 

16.1 

8.95 

1.06577 

66.35 

10.68 

12  2 

6.79 

1.04915 

65.31 

7.97 

16.2 

9.00 

1.06621 

66.38 

10.75 

L2.3 

6.85 

1.04957 

65.34 

8.04 

16.3 

9.06 

1.06664 

66.40 

10.82 

12.4 

6.90 

1.04999 

65.36 

8.10 

16.4 

9.11 

1.06707 

66.43 

10.89 

12.5 

6.96 

1.05041 

65.39 

8.17 

16.5 

9.17 

1.06751 

66.46 

10.97 

12.6 

7.02 

1.05084 

65.42 

8.24 

16.6 

9.22 

1.06794 

66.48 

11.04 

12.7 

7.07 

1.05126 

65.44 

8.31 

16.7 

9.28 

1.06837 

66.51 

11.11 

12.8 

7.13 

1.05168 

65.47 

8.38 

16.8 

9.33 

1.06881 

66.54 

11.18 

12.9 

7.18 

1.05210 

65.50 

8.45 

16.9 

9.39 

1.06924 

66.56 

11.25 

13.0 

7.24 

1.05252 

65.52 

8.52 

17.0 

9.45 

1.06968 

66.59 

11.32 

13.1 

7.29 

1.05295 

65.55 

8.59 

17  1 

9.50 

1.07011 

66.62 

11.39 

13.2 

7.35 

1.05337 

65.58 

8.66 

17.2 

9.56 

1.07055 

66.65 

11.46 

13  3 

7.40 

1.05379 

65.60 

8.72 

17.3 

9.61 

1.07098 

66.67 

11.53 

13.4 

7.46 

1.05422 

65.63 

8.79 

17.4 

9.67 

1.07142 

66.70 

11.61 

13.5 

7.51 

1.05464 

65.65 

8.86 

17.5 

9.72 

1.07186 

66.73 

11.68 

13.6 

7.57 

1.05506 

65.68 

8.93 

17.6 

9.78 

1.07229 

66.75 

11.74 

13.7 

7.62 

1.05549 

65.71 

9.00 

17.7 

9.83 

1.07273 

66.78 

11.82 

13.8 

7.68 

1.05591 

65.73 

9.07 

17.8 

9.89 

1.07317 

66.81 

11.89 

13.9 

7.73 

1.05634 

65.76 

9.14 

17.9 

9.94 

1.07361 

66.84 

11.96 

14.0 

7.79 

1.05677 

65.79 

9.21 

18.0 

10.00 

1.07404 

66.86 

12.03 

14  1 

7.84 

1.05719 

65.81 

9.28 

18.1 

10.05 

1.07448 

66.89 

12.11 

14.2 

7.90 

1.05762 

65.84 

9.35 

18.2 

10.11 

1.07492 

66.92 

12.18 

14.3 

7.96 

1.05804 

65.87 

9.42 

18.3 

10.16 

1.07536 

66.95 

12.25 

14.4 

8.01 

1.05847 

65.89 

9.49 

18.4 

10.22 

1.07580 

66.97 

12.32 

14.5 

8.07 

.05890 

65.92 

9.56 

18.5 

10.27 

1.07624 

67.00 

12.40 

14.6 

8.12 

.05933 

65.95 

9.63 

18.6 

10  33 

1.07668 

67.03 

12.47 

14.7 

8.18 

.05975 

65.97 

9.70 

18.7 

10.38 

1.07712 

67.06 

12.54 

14.8 

8.23 

.06018 

66.00 

9.77 

18.8 

10.44 

1.07756 

67.08 

12.61 

14.9 

8.29 

.06061 

66.03 

9.84 

18.9 

10.49 

1.07800 

67.11 

12.68 

15.0 

8.34 

.06104 

66.05 

9.91 

19.0 

10.55 

1.07844 

67.14 

12.76 

15  1 

8.40 

.06147 

66.08 

9.98 

19.1 

10.60 

1.07888 

67.17 

12.83 

15.2 

8.45 

.06190 

66.11 

10.05 

19.2 

10.66 

1.07932 

67.19 

12.90 

15.3 

8.51 

.06233 

66.13 

10.12 

19.3 

10.71 

1.07977 

67.22 

12.97 

15.4 

8.56 

.06276 

66.16 

10.19 

19.4 

10.77 

1.08021 

67.25 

13.05 

15  5 

8.62 

.06319 

66.19 

10.26 

19.5 

10.82 

1.08065 

67.28 

13.12 

15.6 

8.67 

.06362 

66.21 

10.33 

19.6 

10.88 

1.08110 

67.30 

13.19 

15.7 

8.73 

.06405 

66.24 

10.40 

19.7 

10.93 

1.08154 

67.33 

13.26 

15.8 

8.78 

.06448 

66.27 

10.47 

19.8 

10.99 

1.08198 

67.36 

13.34 

15  9 

8.84 

.06491 

66.29 

10.54 

19.9 

11.04 

1.08243 

67.39 

13.41 

204 


METHODS  OF  ANALYSIS 


TABLE  1— Continued 


Degrees 
Brix  or 

%  Suga 
by  Wt. 

Degrees 
Baume, 
Modulu 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub 
per 
Cu.  Ft. 

Degrees 
Brix  or 
%  Suga 
by  Wt. 

Degrees 
Baume, 
Modulu 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 

Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

20.0 

11.10 

1.08287 

67.41 

13.48 

24.0 

13  .  29 

1  .  10092 

68.54 

16.45 

20.1 

11.15 

1.08332 

67.44 

13.56 

24.1 

13.35 

1.10137 

68.57 

16.52 

20.2 

11.21 

1.08376 

67.47 

13.63 

24.2 

13.40 

1.10183 

68.60 

16.60 

20.3 

11.26 

1.08421 

67.50 

13.70 

24.3 

13.46 

1  .  10229 

68.63 

16.67 

20.4 

11.32 

1.08465 

67.52 

13.77 

24.4 

13.51 

1  .  10275 

68.66 

16.75 

20.5 

11.37 

1.08510 

67.55 

13.85 

24.5 

13.57 

1  .  10321 

68.69 

16.83 

20.6 

11.43 

1.08554 

67.58 

13.92 

24.6 

13.62 

1  .  10367 

68.72 

16.90 

20.7 

11.48 

1.08599 

67.60 

13.99 

24.7 

13.67 

1  .  10413 

68.75 

16.98 

20.8 

11.54 

1.08644 

67.64 

14.07 

24.8 

13.73 

1  .  10459 

68.78 

17.05 

20.9 

11.59 

1.08689 

67.66 

14.14 

24.9 

13.78 

1  .  10505 

68.80 

17.13 

21.0 

11.65 

1.08733 

67.69 

14.21 

25.0 

13.84 

1  .  10551 

68.82 

17.21 

21.1 

11.70 

1.08778 

67.72 

14.29 

25.1 

13.89 

1  .  10597 

68.85 

17.28 

21.2 

11.76 

1.08823 

67  .-75 

14.36 

25.2 

13.95 

1  .  10643 

68.88 

17.36 

21.3 

11.81 

1.08868 

67.78 

14.43 

25.3 

14.00 

1  .  10689 

68.91 

17.43 

21.4 

11.87 

1.08913 

67.80 

14.51 

25.4 

14.06 

1  .  10736 

68.94 

17.51 

21.5 

11.92 

1.08958 

67.83 

14.58 

25.5 

14.11 

1  .  10782 

68.97 

17.59 

21.6 

11.98 

1.09003 

67.86 

14.66 

25.6 

14.17 

1  .  10828 

69.00 

17.66 

21.7 

12.03 

1.09048 

67.89 

14.73 

25.7 

14.22 

1  .  10874 

69.03 

17.74 

21.8 

12.09 

1.09093 

67.92 

14.81 

25.8 

14.28 

1  .  10921 

69.06 

17.82 

21.9 

12.14 

1.09138 

67.94 

14.88 

25.9 

14.33 

1  .  10967 

69.08 

17.89 

22.0 

12.20 

1.09183 

67.97 

14.95 

26.0 

14.39 

1.11014 

69.11 

17.97 

22.1 

12.25 

1.09228 

68.00 

15.03 

26.1 

14.44 

1.11060 

69.14 

18.05 

22.2 

12.31 

1.09273 

68.03 

15.10 

26.2 

14.49 

1.11106 

69.17 

18.12 

22.3 

12.36 

1.09318 

68.06 

15.18 

26.3 

14.55 

1.11153 

69.20 

18.20 

22.4 

12.42 

1.09364 

68.08 

15.25 

26.4 

14.60 

•1.11200 

69.23 

18.28 

22.5 

12.47 

1.09409 

68.11 

15.32 

26.5 

14.66 

1.11246 

69.26 

18.35 

22.6 

12.52 

1.09454 

68.14 

15.40 

26.6 

14.71 

1.11293 

69.20 

18.43 

22.7 

12.58 

1.09499 

68.17 

15.47 

26.7 

14.77 

1.11339 

69.32 

18.51 

22.8 

12.63 

1.09545 

68.20 

15.55 

26.8 

14.82 

1.11386 

69.34 

18.58 

22.9 

12.69 

1.09590 

68.23 

15.62 

26.9 

14.88 

1.11433 

69.37 

18.66 

23.0 

12.74 

1.09636 

68.26 

15.70 

27.0 

14.93 

1.11480 

69.40 

18.74 

23.1 

12.80 

1.09681 

68.28 

15.77 

27.1 

14.99 

1.11526 

69.43 

18.82 

23.2 

12.85 

1.09727 

68.31 

15.84 

27.2 

15.04 

1.11573 

69.46 

18.89 

23.3 

12.91 

1.09772 

68.34 

15.92 

27.3 

15.09 

1.11620 

69.49 

18.97 

23.4 

12.96 

1.09818 

68.37 

16.00 

27.4 

15.15 

1.11667 

69.52 

19.05 

23.5 

13.02 

1.09863 

68.40 

16.07 

27.5 

15.20 

1.11714 

69.55 

19.13 

23.6 

13.07 

1.09909 

68.43 

16.14 

27.6 

15.26 

1.11761 

69.58 

19.20 

23.7 

13.13 

1.09954 

68.46 

16.22 

27.7 

15.31 

1.11808 

69.61 

19.29 

23.8 

13.18 

1.10000 

68.49 

16.30 

27.8 

15.37 

1.11855 

69.64 

19.36 

23.9 

13.24 

1.10046 

68.52 

16.38 

27.9 

15.42 

1.11902 

69.67 

19.44 

XXVII.       TABLES 


205 


TABLE  1— Continued 


Degrees 
Brix  or 
%  Sugar 
by  Wt. 

degrees 
3aume, 
Modulus 
145 

Specific 
Gravity 
at 
0°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

degrees 
Brix  or 
Jo  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
0°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

28.0 

15.48 

1.11949 

69.70 

19.52 

32.0 

17.65 

1.13861 

70.89 

22.68 

28  1 

15.53 

1.11996 

69.72 

19.59 

32.1 

17.70 

1.13909 

70.92 

22.77 

28.2 

15.59 

1.12043 

69.75 

19.67 

32.2 

17.76 

1  .  13958 

70.95 

22.85 

28.3 

15.64 

1.12090 

69.78 

19.75 

32.3 

17.81 

1  .  14006 

70.98 

22.93 

28.4 

15.69 

1  .  12138 

69.81 

19.82 

32.4 

17.87 

1.14055 

71.01 

23.01 

28.5 

15.75 

1  .  12185 

69.84 

19.90 

32.5 

17.92 

1.14103 

71.04 

23.09 

28.6 

15.80 

1.12232 

69.87 

19.98 

32.6 

17.98 

1.14152 

71.07 

23.17 

28.7 

15.86 

1.12280 

69.90 

20.06 

32.7 

18.03 

1  .  14201 

71.10 

23.25 

28.8 

15.91 

1.12327 

69.93 

20.14 

32.8 

18.08 

1.14250 

71.13 

23.33 

28.9 

15.97 

1  .  12374 

69.96 

20.22 

32.9 

18.14 

1  .  14298 

71.16 

23.41 

29.0 

16.02 

1  .  12422 

69.99 

20.30 

33.0 

18.19 

1.14347 

71.19 

23.49 

29.1 

16.08 

1  .  12469 

70.02 

20.38 

33.1 

18.25 

1.14396 

71.22 

23.57 

29.2 

16.13 

1.12517 

70.05 

20.45 

33.2 

18.30 

1  .  14445 

71.25 

23.66 

29.3 

16.18 

1.12564 

70.08 

20.53 

33.3 

18.36 

1.14494 

71.28 

23.74 

29.4 

16.24 

1.12612 

70.11 

20.61 

33.4 

18.41 

1.14543 

71.31 

23.82 

29.5 

16.29 

1.12659 

70.14 

20.69 

33.5 

18.46 

1  .  14592 

71.34 

23.90 

29.6 

16.35 

1  .  12707 

70.17 

20.77 

33.6 

18.52 

1  .  14641 

71.37 

23.98 

29.7 

16.40 

1  .  12755 

70.20 

20.85 

33.7 

18.57 

1.14690 

71.40 

24.06 

29.8 

16.46 

1.12802 

70.23 

20.93 

33.8 

18.63 

1  .  14739 

71.43 

24.14 

29.9 

16.51 

1  .  12850 

70.26 

21.01 

33.9 

18.68 

1.14788 

71.46 

24.22 

30.0 

16.57 

1.12898 

70.29 

21.08 

34.0 

18.73 

1.14837 

71.50 

24.31 

30.1 

16.62 

1.12946 

70.32 

21.17 

34.1 

18.79 

1  .  14886 

71.53 

24.39 

30.2 

16.67 

1.12993 

70.35 

21.25 

34.2 

18.84 

1  .  14936 

71.56 

24.47 

30.3 

16.73 

1  13041 

70.38 

21.32 

34.3 

18.90 

1  .  14985 

71.59 

24.56 

30.4 

16.78 

1.13089 

70.41 

21.40 

34.4 

18.95 

1.15034 

71.62 

24.64 

30.5 

16.84 

1.13137 

70.44 

21.48 

34.5 

19.00 

1.15084 

71.65 

24.72 

30.6 

16.89 

1.13185 

70.47 

21.56 

34.6 

19.06 

1.15133 

71.68 

24.80 

30.7 

16.95 

1.13233 

70.50 

21.64 

34.7 

19.11 

1.15183 

71.71 

24.88 

30.8 

17.00 

1.13281 

70.53 

21.72 

34.8 

19.17 

1  .  15232 

71.74 

24.97 

30.9 

17.05 

1.13329 

70.56 

21.80 

34.9 

19.22 

1  .  15282 

71.77 

25.05 

31.0 

17.11 

1  .  13378 

70.59 

21.88 

35.0 

19.28 

1.15331 

71.80 

25.13 

31.1 

17.16 

1.13426 

70.62 

21.96 

35.1 

19.33 

1.15381 

71.83 

25.21 

31.2 

17.22 

1.13474 

70.65 

22.04 

35.2 

19.38 

1.15430 

71.86 

25.29 

31.3 

17  27 

1.13522 

70.68 

22.12 

35.3 

19.44 

1  .  15480 

71.89 

25.38 

31.4 

17.33 

1.13570 

70.71 

22.20 

35.4 

19.49 

1  .  15530 

71.93 

25.46 

31  .  5 

17.38 

1.13619 

70.74 

22.28 

35.5 

19.55 

1.15579 

71.96 

25.55 

31.6 

17.43 

1.13667 

70.77 

22.36 

35.6 

19.60 

1.1562 

71.99 

25.63 

31.7 

17.49 

1.13715 

70.80 

22.44 

35.7 

19.65 

1.1567 

72.02 

25.71 

31.8 

17.54 

1.13764 

70.83 

22.52 

35.8 

19.71 

1  .  1572 

72.05 

25.79 

31.9 

17.60 

1.13812 

70.86 

22.60 

35.9 

19.76 

1.1577 

72.08 

25.88 

206 


METHODS  OF  ANALYSIS 


TABLE  1— Continued 


Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 

at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub 
per 
Cu.  Ft. 

Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

36.0 

19.81 

1.15828 

72.11 

25.96 

40.0 

21.97 

1.17853 

73.37 

29.35 

36.1 

19.87 

1.15878 

72.  14 

26.04 

40.1 

22.02 

1  .  17904 

73.41 

29.44 

36.2 

19.92 

1  .  15928 

72.18 

26  .  13 

40.2 

22.07 

1.17956 

73.44 

29.52 

36.3 

19.98 

1  .  15978 

72.21 

26.21 

40.3 

22.13 

1.18007 

73.47 

29.61 

36.4 

20.03 

1  .  16028 

72.24 

26.30 

40.4 

22.18 

1  .  18058 

73.50 

29.69 

36.5 

20.08 

1  .  16078 

72.27 

26.38 

40.5 

22.23 

1.18110 

73.53 

29.78 

36.6 

20.14 

1  16128 

72.30 

26.46 

40.6 

22.29 

1  .  18162 

73.57 

29.87 

36.7 

20.19 

1.16178 

72.33 

26.55 

40.7 

22.34 

1  .  18213 

73.60 

29.96 

36.8 

20.25 

1.16228 

72.36 

26.63 

40.8 

22.39 

1  .  18265 

73.63 

30.04 

36.9 

20.30 

1  .  16279 

72.39 

26.71 

40.9 

22.45 

1  .  18316 

73.66 

30.13 

37.0 

20.35 

1  .  16329 

72.42 

26.80 

41.0 

22.50 

1  .  18368 

73.70 

30.22 

37.1 

20.41 

1  .  16379 

72.46 

26.88 

41.1 

22.55 

1  .  18420 

73.73 

30.30 

37.2 

20.46 

1  .  16430 

72.49 

26.97 

41.2 

22.61 

1  .  18472 

73.76 

30.39 

37.3 

20.52 

1  .  16480 

72.52 

27.05 

41.3 

22.66 

1  .  18524 

73.79 

30.48 

37.4 

20.57 

1  .  16530 

72.55 

27.13 

41.4 

22  .  72 

1  .  18575 

73.82 

30.56 

37.5 

20.62 

1  .  16581 

72.58 

27.22 

41.5 

22.77 

1  .  18627 

73.86 

30.65 

37.6 

20.68 

1.16631 

72.61 

27.30 

41.6 

22.82 

1  .  18679 

73.89 

30.74 

37.7 

20.73 

1  .  16682 

72.65 

27.39 

41.7 

22.88 

1.18731 

73.92 

30.82 

37.8 

20.78 

1  .  16732 

72.68 

27.47 

41.8 

22.93 

1  .  18783 

73.95 

30.91 

37.9 

20.84 

1  .  16783 

72.71 

27.56 

41.9 

22.98 

1  .  18835 

73.99 

31.00 

38.0 

20.89 

1  .  16833 

72.74 

27.64 

42.0 

23.04 

1  .  18887 

74.02 

31.09 

38.1 

20.94 

.16884 

72.77 

27.73 

42.1 

23.09 

1  .  18939 

74.05 

31.18 

38.2 

21.00 

.  16934 

72.80 

27.81 

42.2 

23.14 

1  .  18992 

74.08 

31.26 

38.3 

21.05 

.16985 

72.83 

27.89 

42.3 

23.20 

1  .  19044 

74.12 

31.35 

38.4 

21.11 

.17036 

72.87 

27.98 

42.4 

23.25 

1  .  19096 

74.15 

31.44 

38.5 

21.16 

.  17087 

72.90 

28.07 

42.5 

23.30 

1  .  19148 

74.18 

31.53 

38.6 

21.21 

.17138 

72.93 

28.15 

42.6 

23.36 

1  .  19201 

74.21 

31.61 

38.7 

21.27 

.17188 

72.96 

28.24 

42.7 

23.41 

1  .  19253 

74.24 

31.70 

38.8 

21.32 

1  .  17239 

72.99 

28.32 

42.8 

23.46 

1  .  19305 

74.28 

31.79 

38.9 

21.38 

1  .  17290 

73.02 

28.40 

42.9 

23.52 

1  .  19358 

74.31 

31.88 

39.0 

21.43 

1.17341 

73.06 

28.49 

43.0 

23.57 

1.19410 

74.34 

31.97 

39.1 

21.48 

1  .  17392 

73.09 

28.58 

43.1 

23.62 

1  .  19463 

74.38 

32.06 

39.2 

21.54 

1  .  17443 

73.12 

28.66 

43.2 

23.68 

1.19515 

74.41 

32.15 

39.3 

21.59 

1  .  17494 

73.15 

28.75 

43.3 

23.73 

1  .  19568 

74.44 

32.23 

39.4 

21.64 

1  .  17545 

73.18 

28.83 

43.4 

23.78 

1  .  19620 

74.48 

32.32 

39.5 

21.70 

1.17596 

73.21 

28.92 

43.5 

23.84 

1  .  19673 

74.51 

32.41 

39.6 

21.75 

1  .  17648 

73  .  25 

29.01 

43  6 

23.89 

1.19726 

74.54 

32  .  50 

39.7 

21.80 

1  .  17699 

73.28 

29.09 

43.7 

23.94 

1.19778 

74.57 

32.59 

39.8 

21.86 

1  .  17750 

73.31 

29.18 

43.8 

24.00 

1.19831 

74.61 

32.68 

39.9 

21.91 

1  .  17802 

73.34 

29.26 

43.9 

24.05 

1  .  19884 

74.64 

32.77 

XXVII.       TABLES 


207 


TABLE  1— Continued 


Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

44.0 

24.10 

.19936 

74.67 

32.86 

48.0 

26.23 

1.22080 

76.01 

36.48 

44.1 

24.16 

.19989 

74.71 

32.95 

48.1 

26.28 

1.22134 

76.04 

36.58 

44.2 

24.21 

.20042 

74.74 

33.04 

48.2 

26.33 

1.22189 

76.08 

36.67 

44.3 

24.26 

.20095 

74.77 

33.12 

48.3 

26.38 

1.22243 

76.11 

36.76 

44.4 

24.32 

.20148 

74.80 

33.21 

48.4 

26.44 

1.22298 

76.14 

36.85 

44.5 

24.37 

1.20201 

74.84 

33.30 

48.5 

26.49 

1.22352 

76.18 

36.95 

44.6 

24.42 

1.20254 

74.87 

33.39 

48.6 

26.54 

1.22406 

76.21 

37.04 

44.7 

24.48 

1.20307 

74.90 

33.48 

48.7 

26.59 

1.22461 

76.24 

37.13 

44.8 

24.53 

1.20360 

74.94 

33.57 

48.8 

26.65 

1.22516 

76.28 

37.22 

44.9 

24.58 

1.20414 

74.97 

33.66 

48.9 

26.70 

1.22570 

76.31 

37.32 

45.0 

24.63 

.20467 

75.00 

33.75 

49.0 

26.75 

.22625 

76.35 

37.41 

45.1 

24.69 

.20520 

75.04 

33.84 

49.1 

28.81 

.22680 

76.38 

37.50 

45.2 

24.74 

.20573 

75.07 

33.93 

49.2 

26.86 

.22735 

76.41 

37.59 

45.3 

24.79 

.20627 

75.11 

34.02 

49.3 

26.91 

.22789 

76.45 

37.68 

45.4 

24.85 

.20680 

75.14 

34.11 

49.4 

26.96 

.22844 

76.48 

37.78 

45.5 

24.90 

.20733 

75.17 

34.20 

49.5 

27.02 

.22899 

76.52 

37.87 

45.6 

24.95 

.20787 

75.20 

34.29 

49.6 

27.07 

.22954 

76.55 

37.97 

45.7 

25.01 

.20840 

75.24 

34.38 

49.7 

27.12 

.23009 

76.59 

38.07 

45.8 

25.06 

.20894 

75.27 

34.47 

49.8 

27.18 

.23064 

76.62 

38.16 

45.9 

25  11 

.20947 

75.30 

34.56 

49.9 

27.23 

.23119 

76.66 

38.25 

46.0 

25.17 

.21001 

75.33 

34.65 

50.0 

27.28 

.23174 

76.69 

38.35 

46.1 

25.22 

.21054 

75.37 

34.74 

50.1 

27.33 

.23229 

76.72 

38.43 

46.2 

25.27 

.21108 

75.40 

34.83 

50.2 

27.39 

.23284 

76.76 

38.53 

46.3 

25.32 

.21162 

75.43 

34.92 

50.3 

27.44 

.23340 

76.79 

38.63 

46.4 

25.38 

.21215 

75.47 

35.02 

50.4 

27.49 

.23395 

76.83 

38.72 

46.5 

25.43 

.21269 

75.50 

35.11 

50.5 

27.54 

.23450 

76.86 

38.81 

46.6 

25.48 

.21323 

75.53 

35.20 

50.6 

27.60 

.23506 

76.90 

38.91 

46.7 

25.54 

.21377 

75.57 

35.29 

50.7 

27.65 

.23561 

76.93 

39.00 

46.8  - 

25.59 

.21431 

75.60 

35.38 

50.8 

27.70 

.23616 

76.97 

39.09 

46.9 

25.64 

.21484 

75.63 

35.47 

50.9 

27.75 

.23672 

77.00 

39.19 

47.0 

25.70 

.21538 

75.67 

35.56 

51.0 

27.81 

.23727 

77.03 

39.29 

47.1 

25.75 

.21592 

75.70 

35.65 

51.1 

27.86 

.23782 

77.07 

39.38 

47.2 

25.80 

.21646 

75.73 

35.74 

51.2 

27.91 

.23838 

77.10 

39.47 

47.3 

25.86 

.21700 

75.77 

35.84 

51.3 

27.96 

.23894 

77.13 

39.57 

47.4 

25.91 

.21755 

75.80 

35.93 

51.4 

28.02 

.23949 

77.17 

39.67 

47.5 

25.96 

1.21809 

75.84 

36.02 

51.5 

28.07 

.24005 

77.21 

39.76 

47.6 

26.01 

1.21863 

75.87 

36.11 

51.6 

28.12 

.24060 

77.24 

39.86 

47.7 

26.07 

1.21917 

75.91 

36.21 

51.7 

28.17 

1.24116 

77.28 

39.95 

48.7 

26.12 

1.21971 

75.94 

36.30 

51.8 

28.23 

1.24172 

77.31 

40.05 

47.9 

26.17 

1.22026 

75.97 

36.39 

51.9 

28.28 

1.24228 

77.35 

40.14 

208 


METHODS  OF   ANALYSIS 


TABLE  1— Continued 


Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

Degrees 
Brix  or 

%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

52.0 

28.33 

1.24284 

77.38 

40.24 

56.0 

30.42 

1.26548 

78.79 

44.12 

52.1 

28.38 

1.24339 

77.42 

40.34 

56.1 

30.47 

1.26605 

78.83 

44.22 

52.2 

28.44 

1.24395 

77.45 

40.43 

56.2 

30.52 

1.26663 

78.86 

44.32 

52.3 

28.49 

1.24451 

77.49 

40.53 

56.3 

30.57 

1  .  26720 

78.90 

44.42 

52.4 

28.54 

1.24507 

77.52 

40.62 

56.4 

30.63 

1.26778 

78.93 

44.52 

52.5 

28.59 

1.24563 

77.56 

40.72 

56.5 

30.68 

1.26835 

78.97 

44.62 

52.6 

28.65 

1.24619 

77.59 

40.81 

56.6 

30.73 

1.26893 

79.01 

44.72 

52.7 

28.70 

1.24675 

77.63 

40.91 

56.7 

30.78 

1.26950 

79.04 

44.82 

52.8 

28.75 

1.24731 

77.66 

41.00 

56.8 

30.83 

1.27008 

79.08 

44.92 

52.9 

28.80 

1.24788 

77.70 

41.10 

56.9 

30.89 

1.27066 

79.11 

45.01 

53.0 

28.86 

1.24844 

77.73 

41.20 

57.0 

30.94 

1.27123 

79.15 

45.11 

53.1 

28.91 

1.24900 

77.77 

41.29 

57.1 

30.99 

1.27181 

79.19 

45.21 

53.2 

28.96 

1  .  24956 

77.80 

41.39 

57.2 

31.04 

1.27239 

79.22 

45.31 

53.3 

29.01 

1.25013 

77.84 

41.49 

57.3 

31.09 

1.27297 

79.26 

45.42 

53.4 

29.06 

1.25069 

77.87 

41.58 

57.4 

31.15 

1.27355 

79.29 

45.51 

53.5 

29.12 

1.25126 

77.91 

41.68 

57.5 

31.20 

.27413 

79.33 

45.61 

53.6 

29.17 

1.25182 

77.94 

41.78 

57.6 

31.25 

.27471 

79.37 

45.71 

53.7 

29.22 

1.25238 

77.98 

41.87 

57.7 

31.30 

.27529 

79.40 

45.81 

53.8 

29.27 

1.25295 

78.01 

41.97 

57.8 

31.35 

.27587 

79.44 

45.92 

53  9 

29.32 

1.25351 

78.05 

42.07 

57.9 

31.40 

.27645 

79.48 

46.02 

54.0 

29.38 

1.25408 

78.08 

42.16 

58.0 

31.46 

1.27703 

79.51 

46.12 

54.1 

29.43 

1.25465 

78.12 

42.26 

58.1 

31.51 

1.27761 

79.55 

46.22 

54.2 

29.48 

1.25521 

78.15 

42.36 

58.2 

31.56 

1.27819 

79.58 

46.32 

54.3 

29.53 

1.25578 

78.19 

42.46 

58.3 

31.61 

1.27878 

79.62 

46.42 

54.4 

29.59 

1.25635 

78.22 

42.55 

58.4 

31.66 

1.27936 

79.66 

46.52 

54.5 

29.64 

1.25692 

78.26 

42.65 

58.5 

31.71 

1.27994 

79.69 

46.62 

54.6 

29.69 

1.25748 

78.29 

42.75 

58.6 

31.76 

1.28052 

79.73 

46.72 

54.7 

29.74 

1.25805 

78.33 

42.85 

58.7 

31.82 

1.28111 

79.77 

46.82 

54.8 

29.80 

1.25862 

78.36 

42.94 

58.8 

31.87 

1.28169 

79.80 

46.92 

54.9 

29.85 

1.25919 

78.40 

43.04 

58.9 

31.92 

1.28228 

79.84 

47.03 

55.0 

29.90 

.25976 

78.44 

43.14 

59.0 

31.97 

1.28286 

79.88 

47.13 

55.1 

29.95 

.26033 

78.47 

43.24 

59.1 

32.02 

1.28345 

79.91 

47.23 

55.2 

30.00 

.26090 

78.51 

43.34 

59.2 

32.07 

1.28404 

79.95 

47.33 

55.3 

30.06 

.26147 

78.54 

43.43 

59.3 

32.13 

1.28462 

79.99 

47.43 

55.4 

30.11 

.26204 

78.58 

43.53 

59.4 

32.18 

1.28520 

80.02 

47.53 

55.5 

30.16 

1.26261 

78.61 

43.63 

59.5 

32.23 

1.28579 

80.06 

47.64 

55.6 

30.21 

1.26319 

78.65 

43.73 

59.6 

32.28 

1.28638 

80.10 

47.74 

55.7 

30.26 

1.26376 

78.69 

43.83 

59.7 

32.33 

1.28697 

80.13 

47.84 

55.8 

30.32 

1.26433 

78.72 

43.93 

59.8 

32.38 

1.28755 

80.17 

47.94 

55.9 

30.37 

1.26490 

78.76 

44.03 

59.9 

32.43 

1.28814 

80.20 

48.04 

XXVII.       TABLES 


209 


TABLE  1— Continued 


Dogroos 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 

Cubic 
Foot 

Pounds 
Dry  Sub 
per 
Cu.  Ft. 

Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 

Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

60.0 

32.49 

.28873 

80.24 

48.14 

64.0 

34.53 

.31260 

81.73 

52.31 

60.1 

32.54 

.28932 

80.28 

48.25 

64.1 

34.58 

.31320 

81.77 

52.41 

60.2 

32.59 

.28991 

80.31 

48.35 

64.2 

34.63 

.31381 

81.80 

52.52 

60.3 

32.64 

.29050 

80.35 

48.45 

64.3 

34.68 

.31441 

81.84 

52.62 

60.4 

32.69 

29109 

80.39 

48.56 

64.4 

34.74 

.31502 

81.88 

52.73 

60.5 

32.74 

1.29168 

80.43 

48.66 

64.5 

34.79 

.31563 

81.92 

52.84 

60.6 

32.79 

1  .  29227 

80.46 

48.76 

64.6 

34.84 

.31623 

81.96 

52.94 

60.7 

32.85 

1  .  29286 

80.50 

48.86 

64.7 

34.89 

.31684 

81.99 

53.05 

60.8 

32.90 

.29346 

80.54 

48.96 

64.8 

34.94 

.31745 

82.03 

53.16 

60.9 

32.95 

.29405 

80.57 

49.07 

64.9 

34.99 

.31806 

82.07 

53.26 

61.0 

33.00 

.29464 

80.61 

49.17 

65.0 

35.04 

.31866 

82.11 

53.37 

61.1 

33.05 

.29523 

80.65 

49.28 

65.1 

35.09 

.31927 

82.14 

53.47 

61.2 

33.10 

.29583 

80.68 

49.38 

65.2 

35.14 

.31988 

82.18 

53.58 

61.3 

33.15 

.29642 

80.72 

49.48 

65.3 

35.19 

.32049 

82.22 

53.69 

61.4 

33.20 

.29701 

80.76 

49.59 

65.4 

35.24 

.32110 

82.26 

53.80 

61.5 

33.26 

.29761 

80.79 

49.69 

65.5 

35.29 

.32171 

82.30 

53.91 

61.6 

33.31 

.29820 

80.83 

49.79 

65.6 

35.34 

.32232 

82.33' 

54.01 

61.7 

33.36 

.29880 

80.87 

49.90 

65.7 

35.39 

.  32293 

82.37 

54.12 

61.8 

33.41 

.29940 

80.91 

50.00 

65.8 

35.45 

.  32354 

82.41 

54.23 

61.9 

33.46 

.29999 

80.94 

50.10 

65.9 

35.50 

.32415 

82.45 

54.33 

62.0 

33  51 

1.30059 

80.98 

50.21 

66.0 

35.55 

.32476 

82.49 

54.44 

62.1 

33.56 

1.30118 

81.02 

50.31 

66.1 

35.60 

.32538 

82.53 

54.55 

62.2 

33.61 

1.30178 

81.05 

50  .  41 

66.2 

35.65 

1.32599 

82.56 

54.65 

62.3 

33.67 

1.30238 

81.09 

50.52 

66.3 

35.70 

1.32660 

82.60 

54.76 

62.4 

33.72 

1.30298 

81.13 

50.63 

66.4 

35.75 

1  .  32722 

82.64 

54.87 

62.5 

33.77 

.30358 

81.16 

50.73 

66.5 

35.80 

.32783 

82.68 

54.98 

62.6 

33.82 

.30418 

81.20 

50.83 

66.6 

35.85 

.32844 

82.72 

55.09 

62.7 

33.87 

.30477 

81.24 

50.94 

66.7 

35.90 

.  32906 

82.75 

55.19 

62.8 

33.92 

.30537 

81.28 

51.04 

66.8 

35.95 

.32967 

82.79 

55.30 

62  '.• 

33.97 

.30597 

81.32 

51.15 

66.9 

36.00 

.33029 

82.83 

55.41 

63.0 

34.02 

.30657 

81.35 

51.25 

67.0 

36.05 

.33090 

82.87 

55.52 

63.1 

34.07 

.30718 

81.39 

51.36 

67.1 

36.10 

.33152 

82.91 

55.63 

63.2 

34.12 

.30778 

81.43 

51.46 

67.2 

36.15 

.33214 

82.95 

55.74 

63.3 

34.18 

.30838 

81.47 

51.57 

67.3 

36.20 

.33275 

82.98 

55.85 

63.4 

34.23 

.30898 

81.50 

51.67 

67.4 

36.25 

.33337 

83.02 

55.96 

63.5 

34.28 

.30958 

81.54 

51.78 

67.5 

36.30 

.  33399 

83.06 

56.07 

63.6 

34.33 

.31019 

81.58 

51.88 

67.6 

36.35 

.33460 

83.10 

56.18 

63.7 

34.38 

1.31079 

81.62 

51.99 

67.7 

36.40 

.33523 

83.14 

56.29 

63.8 

34.43 

1.31139 

81.65 

52.09 

67.8 

36.45 

.33584 

83.18 

56.40 

63.9 

34.48 

1.31200 

81.69 

52.20 

67.9 

36.50 

1.33646 

83.22 

56.51 

210 


METHODS  OP  ANALYSIS 


TABLE  1— Continued 


Degrees 
Brix  or 

%  Sugar 

Degrees 
Baume, 
Modulus 

Specific 
Gravity 
at 

Pounds 
per 
Cubic 

Pounds 
Dry  Sub. 
per 

Degrees 
Brix  or 

%  Sugar 

Degrees 
Baume, 
Modulus 

Specific 
Gravity 
at 

Pounds 
per 
Cubic 

Pounds 
Dry  Sub. 
per 

by  Wt. 

145 

0°/20°C 

Foot 

Cu.  Ft. 

by  Wt. 

145 

20°/20°C 

Foot 

Cu.  Ft. 

68.0 

36.55 

1.33708 

83.25 

56.61 

72.0 

38.55 

1.36218 

84.82 

61.07 

68.1 

36.61 

1  .  33770 

83.29 

56.72 

72.1 

38.60 

1  .  36282 

84.85 

61.18 

68.2 

36.66 

1.33832 

83.33 

56.83 

72.2 

38.65 

1  .  36346 

84.89 

61.29 

68.3 

36.71 

1.33894 

83.37 

56.94 

72.3 

38.70 

1.36409 

84.93 

61.40 

68.4 

36.76 

1.33957 

83.41 

57.05 

72.4 

38.75 

1.36473 

84.9.7 

61.52 

68.5 

36.81 

1.34019 

83.45 

57.16 

72.5 

38.80 

1  .  36536 

85.02 

61.64 

68.6 

36.86 

1.34081 

83.49 

57.27 

72.6 

38.85 

1.36600 

85.06 

61.75 

68.7 

36.91 

1.34143 

83.52 

57.38 

72.7 

38.90 

1.36664 

85.10 

61.87 

68.8 

36.96 

1.34205 

83.56 

57.49 

72.8 

38.95 

1.36728 

85.14 

61.98 

68.9 

37.01 

1.34268 

83.60 

57.60 

72.9 

39.00 

1.36792 

85.18 

62.10 

69.0 

37.06 

1  .  34330 

83.64 

57.71 

73.0 

39.05 

1.36856 

85.22 

62.21 

69.1 

37.11 

1  .  34392 

83.68 

57.82 

73.1 

39.10 

1.36919 

85.26 

62.33 

69.2 

37.16 

1.34455 

83.72 

57.93 

73.2 

39.15 

1  .  36983 

85.29 

62.43 

69.3 

37.21 

1.34517 

83.76 

58.05 

73.3 

39.20 

1  .  37047 

85.33 

62.55 

69.4 

37.26 

1.34580 

83.80 

58.16 

73.4 

39.25 

1.37111 

85.37 

62.66 

69.5 

37.31 

1.34642 

83,84 

58.27 

73.5 

39.30 

1.37176 

85.42 

62.78 

69.6 

37.36 

1.34705 

83.88 

58.38 

73.6 

39.35 

1.37240 

85.45 

62.89 

69.7 

37.41 

1.34768 

83.91 

58.49 

73.7 

39.39 

1.37304 

85.49 

63.01 

69.8 

37.46 

1.34830 

83.95 

58.60 

73.8 

39.44 

1.37368 

85.53 

63.12 

69.9 

37.51 

1.34893 

83.99 

58.71 

73.9 

39.49 

1.37432 

86.57 

63.24 

70.0 

37.56 

1  .  34956 

84.03 

58.82 

74.0 

39.54 

1  .  37496 

85.61 

63.35 

70.1 

37.61 

1.35019 

84.07 

58.93 

74.1 

39.59 

1.37561 

85.66 

63.47 

70.2 

37.66 

1.35081 

84.11 

59.05 

74.2 

39.64 

1.37625 

85.70 

63.59 

70.3 

37.71 

1.35144 

84.15 

59.16 

74.3 

39.69 

1.37689 

85.74 

63.70 

70.4 

37.76 

1.35207 

84.19 

59.27 

74.4 

39.74 

1.37754 

85.78 

63.82 

70.5 

37.81 

1.35270 

84.23 

59.38 

74.5 

39.79 

1  .  37818 

85.82 

63.94 

70.6 

37.86 

1.35333 

84.26 

59.49 

74.6 

39.84 

1.37883 

85.86 

64.05 

70.7 

37.91 

1.35396 

84.30 

59.60 

74.7 

39.89 

1  .  37947 

85.90 

64.17 

70.8 

37.96 

1.35459 

84.34 

59.71 

74.8 

39.94 

1.38012 

85.94 

64.28 

70.9 

38.01 

1  .  35522 

84.38 

59.83 

74.9 

39.99 

1  .  38076 

85.98 

64.40 

71.0 

38.06 

1.35585 

84.42 

59.94 

75.0 

40.03 

1.38141 

86.02 

64.52 

71.1 

38.11 

1.35648 

84.46 

60.05 

75.1 

40.08 

1  .  38206 

86.06 

64.63 

71.2 

38.16 

1.35711 

84.50 

60.16 

75.2 

40.13 

1.38270 

86.10 

64.75 

71.3 

38.21 

1.35775 

84.54 

60.28 

75.3 

40.18 

1  .  38335 

86.14 

64.86 

71.4 

38.26 

1.35838 

84.58 

60.39 

75.4 

40.23 

1  .  38400 

86.18 

64.98 

71.5 

38.30 

1.35901 

84.62 

60.50 

75.5 

40.28 

1.38465 

86.22 

65.10 

71.6 

38.35 

1.35964 

84.66 

60.62 

75.6 

40.33 

1.38530 

86.26 

65.21 

71.7 

38.40 

1.36028 

84.70 

60.73 

75.7 

40.38 

1  .  38595 

86.30 

65.33 

71.8 

38.45 

1.36091 

84.74 

60.84 

75.8 

40.43 

1.38660 

86.34 

65.45 

71.9 

38.50 

1.36155 

84.78 

60.96 

75.9 

40.48 

1.38725 

86.38 

65.56 

XXVII.      TABLES 


211 


TABLE  1— Continued 


Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

Degrees 
Brix  or 
%  Sugar 
by  Wt, 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 

Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

76.0 

40.53 

1.38790 

86.42 

65.68 

80.0 

42.47 

1.41421 

88.06 

70.45 

76.1 

40.57 

1.38855 

86.46 

65.80 

80.1 

42.52 

1.41488 

88.10 

70.57 

76.2 

40.62 

.38920 

86.50 

65.91 

80.2 

42.57 

1.41554 

88.14 

70.69 

76.3 

40  67 

38985 

86.54 

66.03 

80.3 

42.61 

1.41621 

88.19 

70.82 

76.4 

40.72 

.39050 

86.58 

66.15 

80.4 

42.66 

1.41688 

88.23 

70.94 

76.5 

40.77 

.39115 

86.62 

66.26 

80.5 

42.71 

1.41754 

88.27 

71.06 

76.6 

40.82 

.39180 

86.66 

66.38 

80.6 

42.76 

1.41821 

88.31 

71.18 

76.7 

40.87 

.39246 

86.70 

66.50 

80.7 

42.81 

1.41888 

88.35 

71.30 

76.8 

40.92 

.39311 

86.75 

66.62 

80.8 

42.85 

1.41955 

88.39 

71.42 

76.9 

40.97 

.39376 

86.79 

66.74 

80.9 

42.90 

1.42022 

88.43 

71.54 

77.0 

41.01 

1.39442 

86.83 

66.86 

81.0 

42.95 

1.42088 

88.48 

71.67 

77.1 

41.06 

1.39507 

86.87 

66.98 

81  1 

43.00 

1.42155 

88.52 

71.79 

77.2 

41.11 

1  .  39573 

86.91 

67.09 

81.2 

43.05 

1.42222 

88.56 

71.91 

77.3 

41.16 

1  .  39638 

86.95 

67.21 

81.3 

43.10 

.42289 

88.60 

72.03 

77.4 

41.21 

1.39704 

86.99 

67.33 

81.4 

43.14 

.42356 

88.64 

72.15 

77.5 

41.26 

1.39769 

87.03 

67.45 

81.5 

43.19 

.42423 

88.68 

72.27 

77.6 

41  31 

1.39835 

87.07 

67.57 

81.6 

43.24 

.42490 

88.73 

72.40 

77.7 

41.36 

1.39901 

87.11 

67.68 

81.7 

43.29 

.42558 

88.77 

72.53 

77.8 

41.40 

1.39966 

87.15 

67.80 

81.8 

43.33 

1.42625 

88.81 

72.65 

77.9 

41.45 

1.40032 

87.19 

67.92 

81.9 

43.38 

1.42692 

88.85 

72.77 

78.0 

41.50 

1.40098 

87.24 

68.05 

82.0 

43.43 

1.42759 

88.89 

72.89 

78.1 

41.55 

1.40164 

87.28 

68.17 

82.1 

43.48 

1.42827 

88.94 

73.02 

78.2 

41.60 

1.40230 

87.32 

68.28 

82.2 

43.53 

1.42894 

88.98 

73.14 

78.3 

41.65 

1.40295 

87.36 

68.40 

82.3 

43.57 

1.42961 

89.02 

73.26 

78.4 

41.70 

1  40361 

87.40 

68.52 

82.4 

43.62 

1:43029 

89.06 

73.39 

78.5 

41.74 

1.40427 

87.44 

68.64 

82.5 

43.67 

1.43096 

89.10 

73.51 

78.6 

41  79 

1.40493 

87.48 

68.76 

82.6 

43.72 

.43164 

89.15 

73.64 

78.7 

41.84 

1.40559 

87.52 

68.89 

82.7 

43.77 

.43231 

89.19 

73.76 

78.8 

41.89 

1.40625 

87.56 

69.00 

82.8 

43.81 

.43298 

89.23 

73.88 

78.9 

41.94 

1.40691 

87.61 

69.12 

82.9 

43.86 

.43366 

89.27 

74.00 

79.0 

41.99 

1.40758 

87.65 

69.24 

83.0 

43.91 

.43434 

89.31 

74.13 

79.1 

42.03 

1  40824 

87.69 

69.36 

83.1 

43.96 

.43502 

89.36 

74.26 

79.2 

42.08 

1.40890 

87.73 

69.48 

83.2 

44.00 

.43569 

89.40 

74.38 

79  3 

42.13 

1.40956 

87.77 

69.60 

83.3 

44.05 

.43637 

89.44 

74.50 

79.4 

42.18 

1.41023 

87.81 

69.72 

83.4 

44.10 

.43705 

89.48 

74.63 

79.5 

42.23 

1.41089 

87.85 

69.84 

83.5 

44.15 

.43773 

89.53 

74.76 

79.6 

42.28 

1.41155 

87.89 

69.96 

83.6 

44.19 

.43841 

89.57 

74.88 

79.7 

42.32 

1  41222 

87.93 

70.08 

83.7 

44.24 

.43908 

89.61 

75.00 

79.8 

42.37 

1.41288 

87.98 

70.21 

83.8 

44.29 

.43976 

89.65 

75.13 

79.9 

42.42 

1  41355 

88.02 

70.33 

83.9 

44.34 

.44044 

89.69 

75.25 

METHODS  OF  ANALYSIS 


TABLE  1— Continued 


Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 

Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

Degrees 
Brix  or 

%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft, 

84.0 

44.38 

.44112 

89.74 

75.38 

88.0 

46.27 

.46862 

91.45 

80.48 

84.1 

44.43 

.44180 

89.78 

75.50 

88.1 

46.31 

.46932 

91.49 

80.60 

84.2 

44.48 

.44249 

89.82 

75.63 

88.2 

46.36 

.47002 

91.54 

80.74 

84.3 

44.53 

.44317 

89.86 

75.75 

88.3 

46.41 

.47071 

91.58 

80.87 

84.4 

44.57 

.44385 

89.91 

75.88 

88.4 

46.45 

.47141 

91.62 

80.99 

84.5 

44.62 

.44453 

89.95 

76.01 

88.5 

46.50 

1.47210 

91.67 

81.13 

84.6 

44.67 

.44521 

89.99 

76.13 

88.6 

46.55 

1.47280 

91.71 

81.26 

84.7 

44.72 

1.44590 

90.04 

76.26 

88.7 

46.59 

1.47350 

91.75 

81.38 

84.8 

44.76 

1.44658 

90.08 

76.39 

88.8 

46.64 

1.47420 

91.80 

81.52 

84.9 

44.81 

1.44726 

90.12 

76.51 

88.9 

46.69 

1.47489 

91.84 

81.65 

85.0 

44.86 

1.44794 

90.16 

76.64 

89.0 

46.73 

1.47559 

91.89 

81.78 

85.1 

44.91 

1.44863 

90.21 

76.77 

89.1 

46.78 

1.47629 

91.92 

81.90 

85.2 

44.95 

1.44931 

90.25 

76.89 

89.2 

46.83 

1.47699 

91.97 

82.04 

85.3 

45.00 

1.45000 

90.29 

77.02 

89.3 

46.87 

1.47769 

92.02 

82.17 

85.4 

45.05 

1.45068 

90.33 

77.14 

89.4 

46.92 

1.47839 

92.06 

82.30 

85.5 

45.09 

.45137 

90.38 

77.27 

89.5 

46.97 

.47909 

92.10 

82.43 

85.6 

45.14 

.45205 

90.42 

77.40 

89.6 

47.01 

.47979 

92.15 

82.57 

85.7 

45.19 

.45274 

90.46 

77.52 

89.7 

47.06 

.48049 

92.19 

82.69 

85.8 

45.24 

.45343 

90.50 

77.65 

89.8 

47.11 

.48119 

92.23 

82.82 

85.9 

45.28 

.45411 

90.55 

77.78 

89.9 

47.15 

.48189 

92.28 

82.96 

86.0 

45.33 

.45480 

90.59 

77.91 

90.0 

47.20 

1.48259 

92.32 

83.09 

86.1 

45.38 

.45549 

90.63 

78.03 

90.1 

47.24 

1.48330 

92.37 

83.23 

86.2 

45.42 

.45618 

90.68 

78.17 

90.2 

47.29 

1.48400 

92.41 

83.35 

86.3 

45.47 

.45686 

90.72 

78.29 

90.3 

47.34 

1.48470 

92.45 

83.48 

86.4 

45.52 

.45755 

90.76 

78.42 

90.4 

47.38 

1.48540 

92.49 

83.61 

86.5 

45.57 

.45824 

90.80 

78.54 

90.5 

47.43 

1.48611 

92.54 

83.74 

86.6 

45.61 

.45893 

90.85 

78.68 

90.6 

47.48 

1.48681 

92.58 

83.88 

86.7 

45.66 

.45962 

90.89 

78.80 

90.7 

47.52 

1.48752 

92.63 

84.01 

86.8 

45.71 

.46031 

90.93 

78.93 

90.8 

47.57 

1.48822 

92.67 

84.14 

86.9 

45.75 

.46100 

90.97 

79.05 

90.9 

47.61 

1.48893 

92.72 

84.28 

87.0 

45.80 

1.46170 

91.02 

79.19 

91.0 

47.66 

1.48963 

92.76 

84.41 

87.1 

45.85 

1.46239 

91.06 

79.31 

91.1 

47.71 

1.49034 

92.81 

84.55 

87.2 

45.89 

1.46308 

91.11 

79.45 

91.2 

47.75 

1.49104 

92.85 

84.68 

87.3 

45.94 

1.46377 

91.15 

79.57 

91.3 

47.80 

1.49175 

92.89 

84.82 

87.4 

45.99 

1.46446 

91.19 

79.70 

91.4 

47.84 

1.49246 

92.94 

84.95 

87.5 

46.03 

1.46516 

91.24 

79.84 

91.5 

47.89 

1.49316 

92.98 

85.09 

87.6 

46.08 

1.46585 

91.28 

79.96 

91.6 

47.94 

1.49387 

93.02 

85.22 

87.7 

46.13 

1.46654 

91.32 

80.09 

91.7 

47.98 

1.49458 

93.07 

85.35 

87.8 

46.17 

1.46724 

91.36 

80.21 

91.8 

48.03 

1.49529 

93.11 

85.47 

87.9 

46.22 

1.46793 

91.41 

80.35 

91.9 

48.08 

1.49600 

93.15 

85.60 

XXVII.       TABLES 


213 


TABLE  1— Continued 


Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 
per 
Cubic 
Foot 

Pounds 
Dry  Sub 
per 
Cu.  Ft. 

Degrees 
Brix  or 
%  Sugar 
by  Wt. 

Degrees 
Baume, 
Modulus 
145 

Specific 
Gravity 
at 
20°/20°C 

Pounds 

Cubic 
Foot 

Pounds 
Dry  Sub. 
per 
Cu.  Ft. 

92.0 

48.12 

1.49671 

93.20 

85.74 

96.0 

49.94 

.52535 

94.99 

91.19 

92.1 

48.17 

1.49741 

93.24 

85.87 

96.1 

49.98 

.  52607 

95.03 

91.32 

92.2 

48.21 

1.49812 

93.29 

86.01 

96.2 

50.03 

.  52680 

95.08 

91.46 

92.3 

48.26 

.49883 

93.33 

86.14 

96.3 

50.08 

.52752 

95.12 

91.60 

92.4 

48.30 

.49954 

93.37 

86.27 

96.4 

50.12 

.52824 

95.17 

91.74 

92.5 

48.35 

.50026 

93.42 

86.41 

96.5 

50.16 

1.52897 

95.21 

91.88 

92.6 

48.40 

.50097 

93.47 

86.55 

96.6 

50.21 

1  .  52969 

95.26 

92.02 

92.7 

48.44 

.50168 

93.51 

86.68 

96.7 

50.25 

1  .  53042 

95.30 

92.16 

92.8 

48.49 

.50239 

93  .  55 

86.82 

96.8 

50.30 

1.53114 

95.35 

92.30 

92.9 

48.53 

.50310 

93.60 

86.95 

96.9 

50.34 

1.53187 

95.39 

92.43 

93.0 

48.58 

.  50381 

93.64 

87.09 

97.0 

50.39 

1.53260 

95.44 

92.57 

93.1 

48.62 

.  50453 

93.69 

87.23 

97.1 

50.43 

1.53332 

95.48 

92.71 

§3.2 

48.67 

.50524 

93.73 

87.36 

97.2 

50.48 

1.53405 

95.53 

92.86 

93.3 

48.72 

.50595 

93.77 

87.49 

97.3 

50.52 

.53478 

95.57 

93.00 

93.4 

48.76 

.50667 

93.82 

87.63 

97.4 

50.57 

.53551 

95.62 

93.13 

93.5 

48.81 

.50738 

93.87 

87.77 

97.5 

50.61 

.  53623 

95.66 

93.27 

93.6 

48.85 

.  50810 

93.91 

87.90 

97.6 

50.66 

.  53696 

95.71 

93.41 

93.7 

48.90 

.50881 

93.96 

88.04 

97.7 

50.70 

.  53769 

95.75 

93.55 

93.8 

48.94 

.50952 

94.00 

88.17 

97.8 

50.75 

.53842 

95.80 

93.69 

93.9 

48.99 

.51024 

94.04 

88.30 

97.9 

50.79 

.53915 

95.85 

93.83 

94.0 

49.03 

.51096 

94.09 

88.44 

98.0 

50.84 

.53988 

95.89 

93.97 

94.1 

49.08 

.51167 

94.13 

88.58 

98.1 

50.88 

.54061 

95.94 

94.12 

94.2 

49.12 

1.51239 

94.18 

88.72 

98.2 

50.93 

.54134 

95.98 

94.26 

94.3 

49.17 

1.51311 

94.22 

88.85 

98.3 

50.97 

.54207 

96.03 

94.40 

94.4 

49.22 

1.51382 

94.27 

88.99 

98.4 

51.02 

.  54280 

96.08 

94.54 

94.5 

49.26 

.51454 

94.31 

89.12 

98.5 

51.06 

.54353 

96.12 

94.68 

94.6 

49.31 

.51526 

94.36 

89.26 

•98.6 

51.10 

.54426 

96.17 

94.82 

94.7 

49.35 

.51598 

94.40 

89.40 

98.7 

51.15 

.54499 

96.22 

94.97 

94.8 

49.40 

.51670 

95.45 

89.53 

98.8 

51.19 

.54573 

96.26 

95.11 

94.9 

49.44 

.51742 

94.49 

89.67 

98.9 

51.24 

1.54646 

96.30 

95.25 

95.0 

49.49 

.51814 

94.54 

89.81 

99.0 

51.28 

1  .  54719 

96.35 

95.39 

95.1 

49.53 

.51886 

94.58 

89.95 

99.1 

51.33 

1.54793 

96.40 

95.53 

95.2 

49.58 

.51958 

94.63 

90.09 

99.2 

51.37 

1.54866 

96.44 

95.67 

95.3 

49.62 

.52030 

94.67 

90.22 

99.3 

51.42 

.54939 

96.48 

95.81 

95.4 

49.67 

.52102 

94.72 

90.36 

99.4 

51.46 

.55013 

96.53 

95.95 

95.5 

49.71 

.52174 

94.76 

90.50 

99.5 

51.50 

.  55087 

96".  58 

96.10 

95.6 

49.76 

.52246 

94.81 

90.64 

99.6 

51.55 

.55160 

96.62 

96.24 

95.7 

49.80 

.52318 

94.85 

90.77 

99.7 

51.59 

.55234 

96.66 

96.38 

95.8 

49.85 

.52390 

94.90 

90.91 

99.8 

51.64 

.55307 

96.71 

96.52 

95.9 

49.90 

.52463 

94.94 

91.04 

99.9 

51.68 

.55381 

96.76 

96.66 

100.0 

51.73 

1  .  55454 

96.80 

96.80 

214 


METHODS  OF  ANALYSIS 


TABLE  2 
FACTORS  FOR  CALCULATION  OF  APPARENT  PURITY 

One-tenth  Dilution  Method 


DEGR. 

DEGR. 

BRIX 

.0 

.1 

.2 

.3 

.4 

.5 

.6 

.7 

.8 

.9 

BRIX 

0 

00.00 

286.7 

143.3 

95.49 

71.59 

57.25 

47.69 

40.86 

35.74 

31.76 

0 

1 

28.57 

25.96 

23.79 

21.95 

20.37 

19.01 

17.81 

16.76 

15.82 

14.98 

1 

2 

14.23 

13.55 

12.93 

12.36 

11.84 

11.36 

10.92 

10.51 

10.13 

9.779 

2 

3 

9.449 

9.141 

8.852 

8.580 

8.324 

8.084 

7.856 

7.641 

7.437 

7.243 

3 

4 

7.059 

6.884 

6.718 

6.559 

6.407 

6.263 

6.124 

5.991 

5.864 

5.742 

4 

5 

5.625 

5.513 

5.405 

5.301 

5.200 

5.104 

5.011 

4.921 

4.834 

4.751 

5 

6 

4.669 

4.591 

4.515 

4.442 

4.370 

4.302 

4.235 

4.170 

4.107 

4.046 

6 

7 

3.987 

3.929 

3.873 

3.818 

3.765 

3.713 

3.663 

3.614 

3.566 

3.520 

7 

8 

3.475 

3.430 

3.387 

3.345 

3.304 

3.264 

3.224 

3.186 

3.149 

3.112 

8 

9 

3.076 

3.041 

3.007 

2.973 

2.941 

2.909 

2.877 

2.846 

2.816 

2.787 

9 

10 

2.758 

2.729 

2.701 

2.674 

2.647 

2.621 

2.595 

2.570 

2.545 

2.521 

10 

11 

2.497 

2.473 

2.450 

2.428 

2.406 

2.384 

2.362 

2.341 

2.320 

2.300 

11 

12 

2.280 

2.260 

2.241 

2.221 

2.203 

2.184 

2.166 

2.148 

2.130 

2.113 

12 

13 

2.096 

2.079 

2.063 

2.046 

2.030 

2.014 

1.999 

.983 

1.968 

1.953 

13 

14 

1.938 

1.924 

1.910 

1.895 

1.882 

1.868 

1.854 

.841 

1.828 

1.815 

14 

15 

.802 

1.789 

1.777 

1.764 

1.752 

1.740 

.728 

.717 

1.705 

1.694 

15 

16 

.682 

1.671 

1.660 

1.649 

1.639 

1.628 

.618 

.607 

1.597 

1.587 

16 

17 

.577 

1.567 

1.557 

1.548 

1.538 

.529 

.520 

.510 

1.501 

1.492 

17 

18 

.483 

1.475 

1.466 

1.457 

1.449 

.440 

.432 

.424 

1.416 

1.408 

18 

19 

.400 

1.392 

1.384 

1.376 

1.368 

.361 

.353 

.346 

1.339 

1.331 

19 

20 

.324 

1.317 

1.310 

1.303 

1.296 

.289 

.282 

.276 

1.269 

1.262 

20 

21 

.256 

1.249 

1.243 

1.237 

1.230 

.224 

.218 

.212 

1.206 

1.200 

21 

22 

1.194 

1.188 

1.182 

1.176 

1.171 

.165 

.159 

.154 

1.148 

1.143 

22 

23 

1.137 

1.132 

1.127 

1.121 

1.116 

.111 

.106 

.100 

1.095 

1.090 

23 

24 

1.085 

1.080 

1.076 

1.071 

1.066 

.061 

.056 

.052 

1.047 

1.042 

24 

25 

1.038 

1.033 

1.029 

1.024 

1.020 

1.015 

1.011 

1.006 

1.002 

.998 

25 

.0 

.1 

.2 

.3 

.4 

.5 

.6 

..7 

.8 

.9 

Derivation 


20° 
Let  D=true  sp.  gr.  of  solution  at    ™  (as  in  Table  1) 


20° 
D'  =  apparent  sp.  gr.  of  solution  at  -^  (ratio  of  weights  in  air) 

B  =  degrees  Brix  of  solution 
Then  D'=D  +  .001  (D-l) 

.„      26x100x1.1      28.680 
99.72BD'    =   BD' 


XXVII.      TABI.ES 


215 


TABLE  3 

TEMPERATURE  CORRECTIONS  FOR  BRIX  HYDROMETERS 
STANDARD  TEMPERATURE  20°  C 

From  Bureau  of  Standards,  Circ.  44,  table  11,  based  on  the  determinations  of  Plato.  The 
table  should  be  used  with  caution  and  only  for  approximate  results  when  the  temperature  differs 
much  from  the  standard  temperature  or  from  the  temperature  of  the  surrounding  air. 


DEGREES  BRIX 

TJT\T  P 

TEMP 

L  Hi  all  . 

°c. 

0 

5 

10 

15 

20 

25 

30 

40 

50 

60 

70 

°C. 

SUBTRACT  FROM  THE  OBSERVED 

READING 

0 

.30 

.49 

.65 

.77 

.89 

.99 

1.08 

1.24 

1.37 

1.44 

1.49 

0 

5 

.36 

.47 

.56 

.65 

.73 

.80 

.86 

.97 

1.05 

1.10 

1.14 

5 

10 

.32 

.38 

.43 

.48 

.52 

.57 

.60 

.67 

.72 

.75 

.77 

10 

11 

.31 

.35 

.40 

.44 

.48 

.51 

.55 

.60 

.65 

.68 

.70 

11 

12 

.29 

.32 

.36 

.40 

.43 

.46 

.50 

.54 

.58 

.60 

.62 

12 

13 

.26 

.29 

.32 

.35 

.38 

.41 

.44 

.48 

.51 

.53 

.55 

13 

14 

!24 

.26 

.29 

.31 

.34 

.36 

.38 

.41 

.44 

.46 

.47 

14 

15 

.20 

.22 

.24 

.26 

.28 

.30 

.32 

.34 

.36 

.38 

.39 

15 

16 

.17 

.18 

.20 

.22 

.23 

.25 

.26 

.28 

.29 

.31 

.32 

16 

17 

.13 

.14 

.15 

.16 

.18 

.19 

.20 

.21 

.22 

.23 

.24 

17 

17.5 

.11 

.12 

.12 

.14 

.15 

.16 

.16 

.17 

.18 

.19 

.20 

17.5 

18 

.09 

.10 

.10 

.11 

.12 

.13 

.13 

.14 

.15 

.15 

.16 

18 

19 

.05 

.05 

.05 

.06 

.06 

.06 

.07 

.07 

.08 

.08 

.08 

19 

ADD  TO  THE  OBSERVED  READING 

21 

.04 

.05 

.06 

.06 

.06 

.07 

.07 

.07 

.08 

.08 

.09 

21 

22 

.10 

.10 

.11 

.12 

.12 

.13 

.14 

.15 

.16 

.16 

.16 

22 

23 

.16 

.16 

.17 

.17 

.19 

.20 

.21 

.22 

.24 

.24 

.24 

23 

24 

.21 

.22 

.23 

.24 

.26 

.27 

.28 

.30 

.32 

.32 

.32 

24 

25 

.27 

.28 

.30 

.31 

.32 

.34 

.35 

.38 

.39 

.40 

.39 

25 

26 

.33 

.34 

.36 

.37 

.40 

.40 

.42 

.46 

.47 

.48 

.48 

26 

27 

.40 

.41 

.42 

.44 

.46 

.48 

.50 

.54 

.55 

.56 

.56 

27 

28 

.46 

.47 

.49 

.51 

.54 

.56 

.58 

.61 

.63 

.64 

.64 

28 

29 

.54 

.55 

.56 

.59 

.61 

.62 

.65 

.70 

.71 

.72 

.72 

29 

30 

.61 

.62 

.63 

.66 

.68 

.71 

.73 

.78 

.79 

.80 

.81 

30 

35 

.99 

1.01 

1.02 

1.06 

1.10 

1.13 

1.16 

1.20 

1.22 

1.23 

1.22 

35 

40 

1.42 

1.45 

1.47 

1.51 

1.54 

1.57 

1.60 

1.64 

1.65 

1.66 

1.65 

40 

45 

1.91 

1.94 

1.96 

2.00 

2.03 

2.05 

2.07 

2.10 

2.10 

2.10 

2.08 

45 

50 

2.46 

2.48 

2.50 

2.53 

2.56 

2.57 

2.58 

2.59 

2.58 

2.56 

2.52 

50 

55 

3.05 

3.07 

3.09 

3.12 

3.12 

3.12 

3.12 

3.10 

•3.07 

3.03 

2.97 

55 

60 

3.69 

3.72 

3.73 

3.73 

3.72 

3.70 

3.67 

3.62 

3.57 

3.50 

3.43 

60 

65 

4.4 

4.4 

4.4 

4.4 

4.4 

4.4 

4.3 

4.2 

4.1 

4.0 

3.9 

65 

70 

5.1 

5.1 

5.1 

5.0 

5.0 

5.0 

4.9 

4.8 

4.7 

4.6 

4.4 

70 

75 

6.1 

6.0 

6.0 

5.9 

5.8 

5.8 

5.7 

5.5 

5.4 

5.2 

5.0 

75 

80 

7.1 

7.0 

7.0 

6.9 

6.8 

6.7 

6.6 

6.3 

6.1 

5.9 

5.6 

80 

0 

5 

10 

15 

20 

25 

30 

40 

50 

60 

70 

216 


METHODS  OF  ANALYSIS 


TABLE  3- A 

TEMPERATURE  CORRECTIONS  FOR  BRIX  HYDROMETERS 
STANDARD  TEMPERATURE  20°  C. 
(Condensed  Table) 

This  table  covers  only  the  temperature  range  permissible  in  laboratory  control  work  and  is 
figured  to  the  nearest  .05°  Brix. 


TEMP. 
°C. 

DEGREES  BRIX 

TEMP. 

°C. 

0 

5 

10 

15 

20 

25 

30 

40 

50 

60 

70 

SUBTRACT  FROM  THE  OBSERVED  READING 

15 
16 
17 

18 
19 

.2 
.15 
.15 
.1 
.05 

.2 
.2 
.15 
.1 
.05 

.25 

.2 
.15 
.1 
.05 

.25 
.2 
.15 
.1 
.05 

.3 
.25 

.2 
.1 
.05 

.3 
.25 

.2 
.15 
.05 

.3 
.25 
.2 
.15 
.05 

.35 
.3 
.2 
.15 
.05 

.35 
.3 
.2 
.15 
.1 

.4 
.3 
.25 
.15 
.1 

.4 
.3 
.25 
.15 
.1 

15 
16 
17 

18 
19 

ADD  TO  THE  OBSERVED  READING 

21 
22 
23 
24 
25 

.05 
.1 
.15 

.2 
.25 

.05 
.1 
.15 

.2 
.3 

.05 
.1 
.15 
.25 
.3 

.05 
.1 
.15 
.25 
.3 

.05 
.1 
.2 
.25 
.3 

.05 
.15 
.2 
.25 
.35 

.05 
.15 

.2 
.3 
.35 

.05 
.15 

.2 
.3 
.4 

.15 
.25 
.3 

.4 

.1 
.15 
.25 
.3 

.4 

.1 
.15 
.25 
.3 
.4 

21 
22 
23 
24 
25 

0 

5 

10 

15 

20 

25 

30 

40 

50 

60 

70 

TABLE  4 

TEMPERATURE  CORRECTIONS  FOR  THE  ABBE  SUGAR  REFRACTOMETER 
STANDARD  TEMPERATURE  20°  C. 

From  Stanek's  temperature  correction  table. 


TEMP. 

°C. 

5 

10 

R 
15 

EFRACTOMETER  READING 

TEMP. 
°C. 

20 

30 

40 

50 

60 

70 

75 

SUBTRACT  FROM  THE  OBSERVED  READING 

15 
16 
17 
18 
19 

.25 
.21 
.16 
.11 

.06 

.27 
.23 
.18 
.12 

.07 

.31 

.26 
.20 
.14 

.08 

.31 

.27 
.20 
.14 
.08 

.34 
.29 
.22 
.15 

.08 

.35 
.31 
.23 
.16 
.09 

.36 
.31 
.23 
.16 
.09 

.37 

.32 
.23 
.15 

.08 

.36 
.31 
.20 
.12 

.07 

.36 
.29 
.17 
.09 
.05 

15 

16 
17 

18 
19 

ADD  TO  THE  OBSERVED  READING 

21 
22 
23 
24 
25 

.06 
.12 

.18 
.24 
.30 

.07 
.14 
.20 
.26 
.32 

.07 
.14 
.20 
.26 
.32 

.07 
.14 
.21 
.27 
.34 

.07 
.14 
.21 

.28 
.36 

.07 
.14 
.21 
.28 
.36 

.07 
.15 
.23 
.30 

.38 

.07 
.14 
.21 
.28 
.36 

.07 
.14 
.22 
.29 
.36 

.07 
.14 
.22 
.29 
.37 

21 
22 
23 
24 
25 

5 

10 

15 

20 

30 

40 

50 

60 

70 

75 

XXVII.       TABLES 


217 


TABLE  5 

APPROXIMATE  AMOUNTS  OF  BASIC  LEAD  ACETATE  SOLUTION  (55°  BRIX)  FOR 

VARIOUS  PRODUCTS 

In  clarifying  sugar  factory  juices,  etc.,  with  basic  lead  acetate,  it  is  important  to  add  a  suffi- 
cient amount  but  at  the  same  time  to  avoid  the  influence  which  a  large  excess  of  the  reagent 
has  on  the  polarization.  This  table  is  intended  as  a  general  guide  for  the  amounts  of  the  standard 
basic  lead  acetate  solution  of  55°  Brix  to  be  used  in  clarifying  the  various  products  analyzed. 
The  figures  should  be  regarded  as  only  approximate,  since  variations  in  the  density  or  composition 
of  the  juices  may  require  the  use  of  different  amounts  of  lead  acetate,  but  they  will  hold  for  the 
most  part  under  ordinary  working  conditions. 


KIND  OF  MATERIAL 

AMT.  OF  MATERIAL 

ml  OF  LEAD  ACETATE 

Cossettes  (sugar  detn.) 
Cossette  Juice  (purity  detn.) 
Diffusion  Juice 
Pulp 
Pulp  Water 

26  g 
100ml 
100ml 
100ml 
100ml 

6 
*10 
8-10 
2-4 
1-2 

Lime  Cake,  1st 
Lime  Cake,  2d 
Lime  Sewer 
Lime  Sewer 
Excess  Water 
Sweet  Water 
Filter  Cloth  Wash  Water 
Main  Sewer 

54  g 
54  g 
54  g 
100ml 
100ml 
100ml 
100ml 
100ml 

t3  (exactly) 
t3  (exactly) 
t3  (exactly) 
1-3 
1-3 
2-4 
3  (or  more) 
3 

Thin  Juice 
Thick  Juice 
White  Massecuite 
High  Wash  Syrup 
High  Green  Syrup 

100ml 
100  ml  at  23°  Brix 
100  ml  at  23°  Brix 
100  ml  at  23°  Brix 
100  ml  at  23°  Brix 

2 
3 
3 
3 
5 

Remelt  Massecuite 
Remelt  Sugar 
Sugar  Melter 
Low  Wash  Syrup 
Low  Green  Syrup  (Molasses) 

100  ml  at  23°  Brix 
100  ml  at  23°  Brix 
100  ml  at  23°  Brix 
100  ml  at  23°  Brix 
13  g,  or  100  ml  at  23°  Brix 

6 
1-2 
2 

8-10 
10 

Solution  for  Cooler 
Steffen  Waste  &  Wash  Waters 
Saccharate  Milk  and  Cake  (carbonated) 
Saccharate  Cake  (sugar  detn.) 

50ml 
50ml 
100  ml  at  23°  Brix 
13  g 

3-6 
2-4 
3-5 
3-5 

Dried  Pulp 

12.  6  g 

12-15 

*Use  a  stronger  lead  solution  if  10  ml  of  the  regular  solution  is  insufficient. 
fXo  lead  acetate  is  added  if  the  zinc  nitrate  method  is  used. 


218 


METHODS  OF   ANALYSIS 
TABLE  6 

POLARIZATION  TABLE— 200mm  TUBE,  1/10  DILUTION 
For  Pulp  and  Pulp  Water 


POL. 

GRAMS 

POL. 

GRAMS 

POL. 

GRAMS 

POL. 

GRAMS 

POL. 

GRAMS 

READ- 

SUGAR 

READ- 

SUGAR 

READ- 

SUGAR 

READ- 

SUGAR 

READ- 

SUGAR 

ING 

IN 

ING 

IN 

ING 

IN 

ING 

IN 

ING 

IN 

100ml 

100ml 

100  ml 

100  ml 

100  ml 

.0 

.00 

.0 

.29 

2.0 

.57 

3.0 

.86 

4.0 

1.14 

.1 

.03 

.1 

.31 

2.1 

.60 

31 

.89 

4.1 

.17 

.2 

.06 

.2 

.34 

2.2 

.63 

3.2 

.92 

4.2 

.20 

.3 

.09 

.3 

.37 

2.3 

.66 

3.3 

.94 

4.3 

.23 

.4 

.11 

.4 

.40 

2.4 

.69 

3.4 

.97 

4.4 

.26 

.5 

.14 

1.5 

.43 

2.5 

.72 

3.5 

.00 

4.5 

.29 

.6 

.17 

1.6 

.46 

2.6 

.74 

3.6 

.03 

4.6 

.32 

.7 

.20 

1.7 

.49 

2.7 

.77 

3.7 

.06 

4.7 

.34 

.8 

.23 

1.8 

.51 

2.8 

.80 

3.8 

.09 

4.8 

.37 

.9 

.26 

1.9 

.54 

2.9 

.83 

3.9 

.12 

4.9 

.40 

Formula: — Grams  Sugar  in  100  ml  =  Pol.  Reading x. 286 

TABLE  7 

POLARIZATION  TABLE— 400mm  TUBE,  1/10  DILUTION 
For  Sewer  Water 


POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100  ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 

100  ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100  ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 

IN 
100ml 

.0 

.00 

2.0 

.29 

4.0 

.57 

6.0 

.86 

8.0 

1.14 

.1 

.01 

2.1 

.30 

4.1 

.59 

6.1 

.87 

8.1 

1.16 

.2 

.03 

2.2 

.31 

4.2 

.60 

6.2 

.89 

8.2 

1.17 

.3 

.04 

2.3 

.33 

4.3 

.61 

6.3 

.90 

8.3 

1.19 

.4 

.06 

2.4 

.34 

4.4 

.63 

6.4 

.92 

8.4 

1.20 

.5 

.07 

2.5 

.36 

4.5 

.64 

6.5 

.93 

8.5 

1.22 

.6 

.09 

2.6 

.37 

4.6 

.66 

6.6 

.94 

8.6 

1.23 

.7 

.10 

2.7 

.39 

4.7 

.67 

6.7 

.96 

8.7 

1.24 

.8 

.11 

2.8 

.40 

4.8 

.69 

6.8 

.97 

8.8 

1.26 

.9 

.13 

2.9 

.41 

4.9 

.70 

6.9 

.99 

8.9 

1.27 

.0 

.14 

3.0 

.43 

5.0 

.72 

7.0 

1.00 

9.0 

1.29 

.1 

.16 

3.1 

.44 

5.1 

.73 

7.1 

1.02 

9.1 

1.30 

.2 

.17 

3.2 

.46 

5.2 

.74 

7.2 

1.03 

9.2 

1.32 

.3 

.19 

3.3 

.47 

5.3 

.76 

7.3 

1.04 

9.3 

1.33 

.4 

.20 

3.4 

.49 

5.4 

.77 

7.4 

1.06 

9,4 

1.34 

.5 

.21 

3.5 

.50 

5.5 

.79 

7.5 

1.07 

9.5 

1.36 

.6 

.23 

3.6 

.51 

5.6 

.80 

7.6 

1.09 

9.6 

1.37 

.7 

.24 

3.7 

.53 

5.7 

.82 

7.7 

1.10 

9.7 

1.39 

.8 

.26 

3.8 

.54 

5.8 

.83 

7.8 

1.12 

9.8 

1.40 

.9 

.27 

3.9 

.56 

5.9 

.84 

7.9 

1.13 

9.9 

1.42 

Formula:— Grams  Sugar  in  100  ml  =Polariscope  Reading  x.  143 


XXVII.       TABLES 


219 


TABLE  8 

POLARIZATION  TABLE— 400mm  TUBE,  READ  DIRECT 
For  Condensed  Waters 


POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 

100ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 

100ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100  ml 

.0 

.00 

2.0 

.26 

4.0 

.52 

6.0 

.78 

8.0 

1.04 

.1 

.01 

2.1 

.27 

41 

.53 

6.1 

.79 

8.1 

1  05 

2 

.03 

2.2 

.29 

4.2 

.55 

6.2 

.81 

8.2 

1.07 

3 

.04 

23 

.30 

4.3 

.56 

6.3 

.82 

8.3 

1.08 

.4 

.05 

2.4 

.31 

4.4 

.57 

6.4 

.83 

8.4 

1.09 

.5 

.07 

2.5 

.33 

4.5 

.59 

6.5 

.85 

8.5 

1.11 

.6 

.08 

26 

.34 

4.6 

.60 

6.6 

.86 

8.6 

1  12 

.7 

.09 

2.7 

.35 

4.7 

.61 

6.7 

.87 

8.7 

1.13 

.8 

.10 

2.8 

.36 

4.8 

.62 

6.8 

.88 

8.8 

1  14 

.9 

12 

2.9 

.38 

4.9 

.64 

6.9 

.90 

8.9 

1.16 

10 

.13 

3.0 

.39 

5.0 

.65 

7.0 

.91 

9.0 

1.17 

1.1    . 

.14 

3.1 

.40 

5.1 

.66 

71 

.92 

9.1 

1.18 

1.2 

.16 

3.2 

.42 

5.2 

.68 

7.2 

.94 

9.2 

.20 

13 

.17 

33 

.43 

5.3 

.69 

7.3 

.95 

9.3 

.21 

1.4 

.18 

3.4 

.44 

5.4 

.70 

7.4 

.96 

9.4 

.22 

15 

.20 

3.5 

.46 

5.5 

72 

7.5 

.98 

9.5 

.24 

1.6 

.21 

3.6 

.47 

5.6 

.73 

7.6 

.99 

9.6 

.25 

1.7 

.22 

3.7 

.48 

5.7 

.74 

7.7 

1.00 

9.7 

.26 

1.8 

.23 

3.8 

.49 

5.8 

.75 

7.8 

1.01 

9.8 

.27 

19 

.25 

3.9 

.51 

5.9 

.77 

7.9 

1.03 

9.9 

.29 

Formula: — Grams  Sugar  in  100  ml  =Polariscope  Readingx.13 


220 


METHODS  OF  ANALYSIS 


TABLE  9 
STEFFEN  POLARIZATION  TABLE 


POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100  ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100  ml 

POL. 
READ- 
ING 

GRAMS 
SUGAR 
IN 
100  ml 

.0 

.00 

3.5 

1.82 

7.0 

3.64 

10.5 

5.46 

14.0 

7.28 

.1 

.05 

3.6 

1.87 

7.1 

3.69 

10.6 

5.51 

14.1 

7.33 

.2 

.10 

3.7 

1.92 

7.2 

3.74 

10.7 

5.56 

14.2 

7.38 

.3 

.16 

3.8 

1.98 

7.3 

3.80 

10.8 

5.62 

14.3 

7.44 

.4 

.21 

3.9 

2.03 

7:4 

3.85 

10.9 

5.67 

14.4 

7.49 

.5 

.26 

4.0 

2.08 

7.5 

3.90 

11.0 

5.72 

14.5 

7.54 

.6 

.31 

4.1 

2.13 

7.6 

3.95 

11.1 

5.77 

14.6 

7.59 

.7 

.36 

4.2 

2.18 

7.7 

4.00 

11.2 

5.82 

14.7 

7.64 

.8 

.42 

4.3 

2.24 

7.8 

4.06 

11.3 

5.88 

14.8 

7.70 

.9 

.47 

4.4 

2.29 

7.9 

4.11 

11.4 

5.93 

14.9 

7.75 

1.0 

.52 

4.5 

2.34 

8.0 

4.16 

11.5 

5.98 

15.0 

7.80 

1.1 

.57 

4.6 

2.39 

8.1 

4.21 

11.6 

6.03 

15.1 

7.85 

1.2 

.62 

4.7 

2.44 

8.2 

4.26 

11.7 

6.08 

15.2 

7.90 

1.3 

.68 

4.8 

2.50 

8.3 

4.32 

11.8 

6.14 

15.3 

7.96 

1.4 

.73 

4.9 

2.55 

8.4 

4.37 

11.9 

6.19 

15.4 

8.01 

.5 

.78 

5.0 

2.60 

8.5 

4.42 

12.0 

6.24 

15.5 

8.06 

.6 

.83 

5.1 

2.65 

8.6 

4.47 

12.1 

6.29 

15.6 

8.11 

.7 

.88 

5.2 

2.70 

8.7 

4.52 

12.2 

6.34 

15.7 

8.16 

.8 

.94 

5.3 

2.76 

8.8 

4.58 

12.3 

6.40 

15.8 

8.22 

.9 

.99 

5.4 

2.81 

8.9 

4.63 

12.4 

6.45 

15.9 

8.27 

2.0 

1.04 

5.5 

2.86 

9.0 

4.68 

12.5 

6.50 

16.0 

8.32 

2.1 

.09 

5.6 

2.91 

9.1 

4.73 

12.6 

6.55 

16.1 

8.37 

2.2 

.14 

5.7 

2.96 

9.2 

4.78 

12.7 

6.60 

16.2 

8.42 

2.3 

.20 

5.8 

3.02 

9.3 

4.84 

12.8 

6.66 

16.3 

8.48 

2.4 

.25 

5.9 

3.07 

9.4 

4.89 

12.9 

6.71 

16.4 

8.53 

2.5 

.30 

6.0 

3.12 

9.5 

4.94 

13.0 

6.76 

16.5 

8.58 

2.6 

.35 

6.1 

3.17 

9.6 

4.99 

13.1 

6.81 

16.6 

8.63 

2.7 

.40 

6.2 

3.22 

9.7 

5.04 

13.2 

6.86 

16.7 

8.68 

2.8 

.46 

6.3 

3.28 

9.8 

5.10 

13.3 

6.92 

16.8 

8.74 

2.9 

.51 

6.4 

3.33 

9.9 

5.15 

13.4 

6.97 

16.9 

8.79 

3.0 

.56 

6.5 

3.38 

10.0 

5.20 

13.5 

7.02 

17.0 

8.84 

3.1 

.61 

6.6 

3.43 

10.1 

5.25 

13.6 

7.07 

17.1 

8.89 

3.2 

.66 

6.7 

3.48 

10.2 

5.30 

13.7 

7.12 

17.2 

8.94 

3.3 

.72 

6.8 

3.54 

10.3 

5.36 

13.8 

7.18 

17.3 

9  00 

3.4 

1.77 

6.9 

3.59 

10.4 

5.41 

13.9 

7.23 

17.4 

9.05 

Formula: — Grams  Sugar  in  100  ml=Polariscope  Reading x. 52 


XXVII.      TABLES 


221 


TABLE  10 
INVERT  SUGAR  IN  THICK  JUICES,  SYRUPS,  AND  SOLID  PRODUCTS 

This  table  shows  the  weight  of  material  to  be  used  for  the  determination  of  invert  sugar 
according  to  the  method  described  in  Chapter  I,  6  (a). 


Brix  or 
Dry  Sub. 

Grams 

Brix  or 
Dry  Sub. 

Grams 

Brix  or 
Dry  Sub. 

Grams 

Brix  or 
Dry  Sub. 

Grams 

40.0 

110.0 

55.0 

80.0 

70.0 

62.9 

85.0 

51.8 

.5 

108.6 

.5 

79.3 

.5 

62.4 

.5 

51.5 

41.0 

107.3 

56.0 

78.6 

71.0  . 

62.0 

86.0 

51  2 

.5 

106.0 

.5 

77.9 

.5 

61.5 

.5 

50.9 

42.0 

104.8 

57.0 

77.2 

72.0 

61.1 

87.0 

50.6 

.5 

103.5 

.5 

76.5 

.5 

60.7 

.5 

50.3 

43  0 

102  3 

58.0 

75.9 

73.0 

60.3 

88.0 

50.0 

.5 

101.1 

.5 

75.2 

.5 

59.9 

.5 

49.7 

44.0 

100.0 

59.0 

74.6 

74.0 

59.5 

89.0 

49.4 

.5 

98.9 

.5 

73.9 

.5 

59.1 

.5 

49.2 

45.0 

97.8 

60.0 

73.3 

75.0 

58.7 

90.0 

48.9 

.5 

96.7 

.5 

72.7 

.5 

58.3 

.5 

48.6 

46.0 

95.7 

61.0 

72.1 

76.0 

57.9 

91.0 

48.4 

.5 

94.6 

.5 

71.5 

.5 

57.5 

.5 

48.1 

47.0 

93.6 

62.0 

71.0 

77.0 

57.1 

92.0 

47.8 

.5 

92.6 

.5 

70.4 

.5 

56.8 

.5 

47.6 

48.0 

91.7 

63.0 

69.8 

78.0 

56.4 

93.0 

47.3 

.5 

90.7 

.5 

69.3 

.5 

56.1 

.5 

47  1 

49.0 

89.8 

64.0 

68.7 

79.0 

55.7 

94.0 

46.8 

-5 

88.9 

.5 

68.2 

.5 

55.3 

.5 

46.6 

50.0 

88.0 

65.0 

67.7 

80.0 

55.0 

95.0 

46^ 

.5 

87.1 

.5 

67.2 

.5 

54.6 

.5 

46^1 

51.0 

86.3 

66.0 

66.7 

81.0 

54.3 

96.0 

45.8 

.5 

85.4 

.5 

66.2 

.5 

54.0 

.5 

45.6 

52.0 

84.6 

67.0 

65.7 

82.0 

53.7 

97.0 

45.4 

.5 

83.8 

.5 

65.2 

.5 

53.3 

.5 

45.1 

53.0 

83.0 

68.0 

64.7 

83.0 

53.0 

98.0 

44.9 

.5 

82.3 

.5 

64.2 

.5 

52.7 

.5 

44.7 

54.0 

81.5 

69.0 

63.8 

84.0 

52.4 

99.0 

44.4 

.5 

80.7 

.5 

63.3 

.5 

52.1 

.5 

44.2 

FORMULA :— "Grams" 


4400 
:Brix 


222 


METHODS  OF  ANALYSIS 


TABLE  11 
INVERT  SUGAR  IN  THIN  JUICES 


This  table  shows  the  weight  of  material  to  be  used  for  the  determination  of  invert  sugar  ac 
cording  to  the  method  described  in  Chapter  I,  6  (b). 


Brix  or 
Dry  Sub. 

Grams 

Brix  or 
Dry  Sub. 

Grams 

Brix  or 
Dry  Sub. 

Grams 

Brix  or 
Dry  Sub. 

Grams 

12.0 

183.3 

15.0 

146.7 

18.0 

122.2 

21.0 

104.8 

.1 

181.8 

.1 

145.7 

.1 

121.5 

.1 

104.3 

.2 

180.3 

.2 

144.7 

.2 

120.9 

.2 

103.8 

.3 

178.9 

.3 

143.8 

.3 

120.2 

.3 

103.3 

.4 

177.4 

.4 

142.9 

.4 

119.6 

.4 

102.8 

12.5 

176.0 

15.5 

141.9 

18.5 

118.9 

21.5 

102  .  3 

.6 

174.6 

.6 

141.0 

.6 

118.3 

.6 

101.9 

.7 

173.2 

.7 

140.1 

.7 

117.6 

.7 

101.4 

.8 

171.9 

.8 

139.2 

.8 

117.0 

.8 

100.9 

.9 

170.5 

.9 

138.4 

.9 

116.4 

.9 

100.5 

13.0 

169.2 

16.0 

137.5 

19.0 

115.8 

22.0 

100.0 

.1 

167.9 

.1 

136.6 

.1 

115.2 

.1 

99.5 

.2 

166.7 

.2 

135.8 

.2 

114.6 

.2 

99.1 

.3 

165.4 

.3 

134.9 

.3 

114.0 

.3 

98.7 

.4 

164.2 

.4 

134.1 

.4 

113.4 

.4 

98.2 

13.5 

163.0 

16.5 

133.3 

19.5 

112.8 

22.5 

97.8 

.6 

161.8 

.6 

132.5 

.6 

112.2 

.6 

97.3 

.7 

160.6 

.7 

131.7 

.7 

111.7 

.7 

96.9 

.8 

150.4 

.8 

131.0 

.8 

111.1 

.8 

96.5 

.9 

158.3 

.9 

130.2 

.9 

110.6 

.9 

96.1 

.14.0 

157.1 

17.0 

129.4 

20.0 

110.0 

23.0 

95.7 

.1 

156.0 

.1 

128.7 

.1 

109.5 

.1 

95.2 

.2 

154.9 

.2 

127.9 

.2 

108.9 

.2 

94.8 

.3 

153.8 

.3 

127.2 

.3 

108.4 

.3 

94.4 

.4 

152.8 

.4 

126.4 

.4 

107.8 

.4 

94.0 

14.5 

151.7 

17.5 

125.7 

20.5 

107.3 

23.5 

93.6 

.6 

150  .  7 

.6 

125.0 

.6 

106.8 

.6 

93.2 

.7 

149.7 

.7 

124.3 

.7 

106.3 

.7 

92.8 

.8 

148.6 

.8 

123.6 

.8 

105.8 

.8 

92.4 

.9 

147.7 

.9 

122.9 

.9 

105.3 

.9 

91.9 

FORMULA :— "Grams" 


2200 
:Brix 


XXVII.       TABLES 


223 


TABLE  12 

CUPRIC  OXIDE  TABLE  FOR  OBTAINING  THE  PERCENTAGE  OF  INVERT  SUGAR 

(10  Grams  of  Material) 

Calculated  from  Herzfeld's  Table 


CuO 

mg 

Invert 
Sugar  % 

CuO 
mg 

Invert 
Sugar  % 

CuO 

mg 

Invert 
Sugar  % 

CuO 
mg 

Invert 
Sugar  % 

63 

.05 

150 

.40 

238 

.79 

319 

.16 

69 

.07 

156 

.43 

244 

.82 

325 

.19 

75 

.09 

163 

.45 

250 

.85 

331 

.21 

81 

.11 

169 

.48 

256 

.88 

338 

.24 

88 

.14 

175 

.51 

263 

.90 

344 

.27 

94 

.16 

181 

.53 

269 

.93 

•  350 

.30 

100 

.19 

188 

.56 

275 

.96 

356 

1.33 

106 

.21 

194 

.59 

281 

.99 

363 

1.36 

113 

.24 

200 

.62 

288 

1.02 

369 

1.38 

119 

.27 

206 

.65 

294 

1.05 

375 

1.41 

125 

.30 

213 

.68 

300 

1.07 

381 

1.44 

131 

.32 

219 

.71 

306 

1.10 

388 

1.47 

138 

.35 

225 

.74 

313 

1.13 

394 

1.50 

144 

.38 

231 

.76 

TABLE  13 

CUPRIC  OXIDE  TABLE  FOR  OBTAINING  THE  PERCENTAGE  OF  INVERT  SUGAR 

(5  Grains  of  Material) 

Calculated  from  Baumann's  Table 


CuO 

mg 

Invert 
Sugar  % 

CuO  ' 
mg 

Invert 

Sugar  % 

CuO 
mg 

Invert 

Sugar  % 

CuO 
mg 

Invert 
Sugar.  % 

(44) 

(.04) 

138 

.83 

231 

1.65 

319 

2.44 

50 

.09 

144 

.88 

238 

1.70 

325 

2.50 

56 

.14 

150 

.93 

244 

1.76 

331 

2.56 

63 

.19 

156 

.99 

250 

1.82 

338 

2.62 

69 

.25 

163 

1.04 

256 

1.87 

344 

2.68 

75 

.30 

169 

1.10 

263 

1.93 

350 

2.74 

81 

.35 

175 

1.15 

269. 

1.98 

356 

2.79 

88 

.40 

181 

1.21 

275 

2.04 

363 

2.85 

94 

.45 

188 

1.26 

281 

2.10 

369 

2.91 

100 

.51 

194 

1.31 

288 

2.16 

375 

2.97 

106 

.56 

200 

1.37 

294 

2.21 

381 

3.03 

113 

.61 

206 

1.42 

300 

2.27 

388 

3.09 

119 

.66 

213 

1.48 

306 

2.33 

394 

3.15 

125 

.72 

219 

1.54 

313 

2.39 

400 

3.21 

131 

.77 

225 

1.59 

224 


METHODS  OF   ANALYSIS 


TABLE  14 
GaO  BY  SOAP  SOLUTION  IN  THIN  JUICES 

Calculated  for  the  employment  of  20  ml  of  thin  juice,  and  soap  solution  of  the  strength. 
1  ml  =  .001  g  CaO. 

An  example  will  make  clear  the  use  of  the  table: — 20  ml  of  thin  juice  of  11 .8°  Brix  required 
1.2  ml  of  soap  solution.  From  the  table,  on  the  line  opposite  11.8  in  the  Brix  column,  .041  + 
(.081  x.l)  =  .041 +  .008  =  .049,  which  is  the  "CaO  to  100  Brix." 


NUMBER  OF  MILLILITERS  OF  SOAP  SOLUTION 

BRIX 

BRTX 

1 

2 

3 

4 

5 

6 

7 

8 

9 

10 

-DJ/V-L-A. 

8.0 

.061 

.121 

.182 

.243 

.304 

.364 

.425 

.486 

.547 

.607 

8.0 

.2 

.059 

.118 

.178 

.237 

.296 

.355 

.415 

.474 

.533 

.592 

.2 

.4 

.058 

.116 

.173 

.231 

.289 

.3*7 

.404 

.462 

.520 

.578 

.4 

.6 

.056 

.113 

.169 

225 

.282 

.338 

.395 

.451 

.507 

.564 

.6 

.8 

.055 

.110 

.165 

.220 

.275 

.330 

.385 

.440 

.495 

.550 

.8 

9.0 

.054 

.108 

.161 

.215 

.269 

.323 

.376 

.430 

.484 

.538 

9.0 

.2 

.053 

.105 

.158 

.210 

.263 

.315 

.368 

.421 

.473 

.526 

.2 

.4 

.051 

.103 

.154 

.206 

.257 

.308 

.360 

.411 

.463 

.514 

.4 

.6 

.050 

.101 

.151 

.201 

.251 

.302 

.352 

.402 

.453 

.503 

.6 

.8 

.049 

.098 

.148 

.197 

.246 

.295 

.345 

.394 

.443 

.492 

.8 

10.0 

.048 

.096 

.145 

.193 

.241 

.289 

.337 

.386 

.434 

.482 

10.0 

.2 

.047 

.094 

.142 

.189 

.236 

.283 

.331 

.378 

.425 

.472 

.2 

.4 

.046 

.093 

.139 

.185 

.231 

.278 

.324 

.370 

.417 

.463 

.4 

.6 

.045 

.091 

.136 

.181 

.227 

.272 

.318 

.363 

.408 

.454 

.6 

.8 

.044 

.089 

.133 

.178 

.222 

.267 

.311 

.356 

.400 

.445 

.8 

11.0 

.044 

.087 

.131 

.175 

.218 

.262 

.306 

.349 

.393 

.437 

11.0 

.2 

.043 

.086 

.129 

.171 

.214 

.257 

.300 

.343 

.386 

.428 

.2 

.4 

.042 

.084 

.126 

.168 

.210 

.252 

.294 

.336 

.378 

.421 

.4 

.6 

.041 

.083 

.124 

.165 

.206 

.248 

.289 

.330 

.372 

.413 

.6 

.8 

.041 

.081 

.122 

.162 

.203 

.243 

.284 

.325 

.365 

.406 

.8 

12.0 

.040 

.080 

.120 

.159 

.199 

.239 

.279 

.319 

.359 

.399 

12.0 

.2 

.039 

.078 

.118 

.157 

.196 

.235 

.274 

.313 

.353 

.392 

.2 

.4 

.039 

.077 

.116 

.154 

.193 

.231 

.270 

.308 

.347 

.385 

.4 

,6 

.038 

.076 

.114 

.151 

.189 

.227 

.265 

.303 

.341 

.379 

.6 

.8 

.037 

.074 

.112 

.149 

.186 

.223 

.261 

.298 

.335 

.372 

.8 

13.0 

.037 

.073 

.110 

.147 

.183 

.220 

.256 

.293 

.330 

.366 

13.0 

.2 

.036 

.072 

.108 

.144 

.180 

.216 

.252 

.288 

.325 

.361 

.2 

.4 

.035 

.071 

.106 

.142 

.177 

.213 

.248 

.284 

.319 

.355 

.4 

.6 

.035 

.070 

.105 

.140 

.175 

.210 

.245 

.280 

.314 

.349 

.6 

.8 

.034 

.069 

.103 

.138 

.172 

.206 

.241 

.275 

.310 

.344 

.8 

14.0 

.034 

.068 

.102 

.136 

.169 

.203 

.237 

.271 

.305 

.339 

14.0 

.2 

.033 

.067 

.100 

.134 

.167 

.200 

.234 

.267 

.300 

.334 

.2 

.4 

.033 

.066 

.099 

.132 

.164 

.197 

.230 

.263 

.296 

.329 

.4 

.6 

.032 

.065 

.097 

.130 

.162 

.195 

.227 

.259 

.292 

.324 

.6 

.8 

.032 

.064 

.096 

.128 

.160 

.192 

.224 

.256 

.288 

.320 

.8 

1 

2 

3 

4 

5 

6 

7 

8 

9 

10 

XXVII.       TABLES 


225 


TABLE  14-Continued 


NUMBER  OF  MILLILITERS  OF  SOAP  SOLUTION 

r>r>yv 

TVRTX 

LSlvl-A. 

1 

2 

3 

4 

5 

6 

7 

8 

9 

PM 

10 

jL>xviyv 

15.0 

.032 

.063 

.095 

.126 

.158 

.189 

.221 

.252 

.284 

315 

15.0 

.2 

.031 

.062 

.093 

.124 

.155 

.186 

.217 

.248 

.280 

.311 

.2 

.4 

.031 

.061 

.092 

.123 

.153 

.184 

.214 

.245 

.276 

.306 

.4 

.6 

.030 

.060 

.091 

.121 

.151 

.181 

.212 

.242 

.272 

.302 

.6 

.8 

.030 

.060 

.089 

.119 

.149 

.179 

.209 

.238 

.268 

.298 

.8 

16.0 

.029 

.059 

.088 

.118 

.147 

.176 

.206 

.235 

.265 

.294 

16.0 

.2 

.029 

.058 

.087 

.116 

.145 

.174 

.203 

.232 

.261 

.290 

.2 

.4 

.029 

.057 

.086 

.115 

.143 

.172 

.201 

.229 

.258 

.286 

4 

.6 

.028 

.057 

.085 

.113 

.141 

.170 

.198 

.226 

.255 

.283 

.6 

.8 

.028 

.056 

.084 

.112 

.140 

.168 

.195 

.223 

.251 

.279 

.8 

17.0 

.028 

.055 

.083 

.110 

.138 

.165 

.193 

.221 

.248 

.276 

17.0 

.2 

.027 

.054 

.082 

.109 

.136 

.163 

.191 

.218 

.245 

.272 

.2 

.4 

.027 

.054 

.081 

.108 

.134 

.161 

.188 

.215 

.242 

.269 

.4 

.6 

.027 

.053 

.080 

.106 

.133 

.159 

.186 

.213 

.239 

.266 

.6 

.8 

.026 

.052 

.079 

.105 

.131 

.157 

.184 

.210 

.236 

.262 

.8 

18.0 

.026 

.052 

.078 

.104 

.130 

.156 

.182 

.207 

.233 

.259 

18.0 

.2 

.026 

.051 

.077 

.103 

.128 

.154 

.179 

.205 

.231 

.256 

.2 

.4 

.025 

.051 

.076 

.101 

.127 

.152 

.177 

.203 

.228 

.253 

.4 

.6 

.025 

.050 

.075 

.100 

.125 

.150 

.175 

.200 

.225 

.250 

.6 

.8 

.025 

.049 

.074 

.099 

.124 

.148 

.173 

.198 

.223 

.247 

.8 

19.0 

.024 

.049 

.073 

.098 

.122 

.147 

.171 

.196 

.220 

.245 

19.0 

.2 

.024 

.048 

.073 

.097 

.121 

.145 

.169 

.194 

.218 

.242 

.2 

.4 

.024 

.048 

.072 

.096 

.120 

.144 

.167 

.191 

.215 

.239 

.4 

.6 

.024 

.047 

.071 

.095 

.118 

.142 

.166 

.189 

.213 

.237 

.6 

.8 

.023 

.047 

.070 

.094 

.117 

.140 

.164 

.187 

.211 

.234 

.8 

1 

2 

3 

4 

5 

6 

7 

8 

9 

10 

„  .  ,,    No.  of  ml  of  soap  soln. 
Formula:    "CaO  to  100  Brae" '    2x.9972xBrixxD' 


20° 
Where  D'  is  the  apparent  sp.  gr.  at  — 3-  (ratio  of  weights  in  air). 


226 


METHODS  OP  ANALYSIS 


TABLE  15 
GaO  BY  SOAP  SOLUTION  IN  THICK  JUICE,  MASSECUITE,  MOLASSES,  ETC. 

Calculated  for  the  employment  of  10  ml  of  approximately  23°  Brix  material,  and  soap  solu- 
tion of  the  strength,  1  mU.OOl  g  CaO. 

An  example  will  make  clear  the  use  of  the  table:— 10  ml  of  diluted  molasses  of  23.7°  Brix 
required  8.4  ml  of  soap  solution.  From  the  table,  on  the  line  opposite  23.7  in  the  Brix  column,  .308 
+  (.154 x.l)  =.308 +  .015  =  .323,  which  is  the  "CaO  to  100  Brix." 


NUMBER  OF  MILLILITERS  OF  SOAP  SOLUTION 

BRIX 

BRIX 

1 

2 

3 

4 

5 

6 

7 

8 

•     9 

10 

20.0 

.046 

093 

.139 

.185 

.231 

.278 

.324 

.370 

.417 

.463 

20.0 

.1 

.046 

.092 

.138 

.184 

.230 

.276 

.322 

.368 

.414 

.461 

.1 

.2 

.046 

.092 

.137 

.183 

.229 

.275 

.321 

.366 

.412 

.458 

2 

.3 

.046 

.091 

.137 

.182 

.228 

.273 

.319 

.364 

.410 

.456 

'.3 

.4 

.045 

.091 

.136 

.181 

.227 

.272 

.317 

.363 

.408 

.453 

.4 

20.5 

.045 

.090 

.135 

.180 

.225 

.270 

.316 

.361 

.406 

.451 

20.5 

.6 

.045 

.090 

.135 

.179 

.224 

.269 

.314 

.359 

.404 

.448 

.6 

.7 

.045 

.089 

.134 

.178 

.223 

.268 

.312 

.357 

.401 

.446 

.7 

.8 

.044 

.089 

.133 

.177 

.222 

.266 

.311 

.355 

.399 

.444 

.8 

.9 

.044 

.088 

.132 

.177 

.221 

.265 

.309 

.353 

.397 

.441 

.9 

21.0 

.044 

.088 

.132 

.176 

.220 

.263 

.307 

.351 

.395 

.439 

21.0 

.1 

.044 

.087 

.131 

.175 

.218 

.262 

.306 

.349 

.393 

.437 

.1 

.2 

.043 

.087 

.130 

.174 

.217 

.261 

.304 

.348 

.391 

.435 

.2 

.3 

.043 

.086 

.130 

.173 

.216 

.259 

.303 

.346 

.389 

.432 

.3 

.4 

.043 

.086 

.129 

.172 

.215 

.258 

.301 

.344 

.387 

.430 

.4 

21.5 

.043 

.086 

.128 

.171 

.214 

.257 

.300 

.342 

.385 

.428 

21.5 

.6 

.043 

.085 

.128 

.170 

.213 

.256 

.298 

.341 

.383 

.426 

.6 

.7 

.042 

.085 

.127 

.169 

.212 

.254 

.297 

.339 

.381 

.424 

M 

.     i 

.8 

.042 

.084 

.126 

.169 

.211 

.253 

.295 

.337 

.379 

.422 

.8 

.9 

.042 

.084 

.126 

.168 

.210 

.252 

.294 

.336 

.378 

.420 

.9 

22.0 

.042 

.083 

.125 

.167 

.209 

.250 

.292 

.334 

.376 

.417 

22.0 

.1 

.042 

.083 

.125 

.166 

.208 

.249 

.291 

.332 

.374 

.415 

.1 

.2 

.041 

.083 

.124 

.165 

.207 

.248 

.289 

.331 

.372 

.413 

.2 

.3 

.041 

.082 

.123 

.165 

.206 

.247 

.288 

.329 

.370 

.411 

.3 

.4 

.041 

.082 

.123 

.164 

.205 

.246 

.287 

.327 

.368 

.409 

.4 

22.5 

.041 

.081 

.122 

.163 

.204 

.244 

.285 

.326 

.367 

.407 

22.5 

.6 

.041 

.081 

.122 

.162 

.203 

.243 

.284 

.324 

.365 

.405 

.6 

.7 

.040 

.081 

.121 

.161 

.202 

.242 

.282 

.323 

.363 

.403 

.7 

.8 

.040 

.080 

.120 

.161 

.201 

.241 

.281 

.321 

.361 

.401 

.8 

.9 

.040 

.080 

.120 

.160 

.200 

.240 

.280 

.320 

.360 

.400 

.9 

23.0 

.040 

.080 

.119 

.159 

.199 

.239 

.278 

.318 

.358 

.398 

23.0 

.1 

.040 

.079 

.119 

.158 

.198 

.237 

.277 

.317 

.356 

.396 

.1 

.2 

.039 

.079 

.118 

.158 

.197 

.236 

.276 

.315 

.355 

.394 

.2 

.3 

.039 

.078 

.118 

.157 

.196 

.235 

.274 

.314 

.353 

.392 

.3 

.4 

.039 

.078 

.117 

.156 

.195 

.234 

.273 

.312 

.351 

.390 

.4 

1 

2 

3 

4 

5 

6 

7 

8 

9 

10 

XXVII.      TABLES 


227 


TABLE  15— Continued 


NUMBER  OF  MILLILITERS  OF  SOAP  SOLUTION 

BRIX 

BRIX 

1 

2 

3 

4 

5 

6 

7 

8 

9 

10 

23.5 

.039 

.078 

.117 

.155 

.194 

.233 

.272 

.311 

.350 

.388 

23.5 

.6 

.039 

.077 

.116 

.155 

.193 

.232 

.271 

.309 

.348 

.387 

.6 

.7 

.038 

.077 

.115 

.154 

.192 

.231 

.269 

.308 

.346 

.385 

.7 

.8 

.038 

.077 

.115 

.153 

.192 

.230 

.268 

.306 

.345 

.383 

.8 

.9 

.038 

.076 

.114 

.152 

.191 

.229 

.267 

.305 

.343 

.381 

.9 

24.0 

.038 

.076 

.114 

.152 

.190 

.228 

.266 

.304 

.342 

.379 

24.0 

.1 

.038 

.076 

.113 

.151 

.189 

.227 

.264 

.302 

.340 

.378 

.1 

.2 

.038 

.075 

.113 

.150 

.188 

.226 

.263 

.301 

.339 

.376 

.2 

.3 

.037 

.075 

.112 

.150 

.187 

.225 

.262 

.299 

.337 

.374 

.3 

.4 

.037 

.075 

.112 

.149 

.186 

.224 

.261 

.298 

.335 

.373 

.4 

24i5 

.037 

.074 

.111 

.148 

.185 

.223 

.260 

.297 

.334 

.371 

24.5 

.6 

.037 

.074 

.111 

.148 

.185 

.222 

.259 

.295 

.332 

.369 

.6 

.7 

.037 

.074 

.110 

.147 

.184 

.221 

.257 

.294 

.331 

.368 

.7 

.8 

.037 

.073 

.110 

.146 

.183 

.220 

.256 

.293 

.329 

.366 

.8 

.9 

.036 

.073 

.109 

.146 

.182 

.219 

.255 

.292 

.328 

.364 

.9 

25.0 

.036 

.073 

.109 

.145 

.181 

.218 

.254 

.290 

.327 

.363 

25.0 

.1 

.036 

'.072 

.108 

.144 

.181 

.217 

.253 

.289 

.325 

.361 

.1 

.2 

.036 

.072 

.108 

.144 

.180 

.216 

.252 

.288 

.324 

.360 

.2 

.3 

.036 

.072 

.107 

.143 

.179 

.215 

.251 

.286 

.322 

.358 

.3 

.4 

.036 

.071 

.107 

.143 

.178 

.214 

.250 

.285 

.321 

.356 

.4 

25.5 

.035 

.071 

.106 

.142 

.177 

.213 

.248 

.284 

.319 

.355 

25.5 

.6 

.035 

.071 

.106 

.141 

.177 

.212 

.247 

.283 

.318 

.353 

.6 

.7 

.035 

.070 

.106 

.141 

.176 

.211 

.246 

.282 

.317 

.352 

.7 

.8 

.035 

.070 

.105 

.140 

.175 

.210 

.245 

.280 

.315 

.350 

.8 

.9 

.035 

.070 

.105 

.140 

.174 

.209 

.244 

.279 

.314 

.349 

.9 

1 

2 

3 

4 

5 

6 

7 

8 

9 

10 

Formula:     "CaO  to  100  Brix" 


No.  of  ml  of  soap  soln. 
2x.9972xBnxxD' 

20° 


Where  D'  is  the  apparent  sp.  gr.  at  — ^  (ratio  of  weights  in  air). 


228 


METHODS  OF  ANALYSIS 


TABLE  16 
TABLE  FOR  USE  IN  DRY  SUBSTANCE  DETERMINATIONS  ON  PULP  SOLD 

See  Chap.  VI,  3  (b)  for  the  derivation  and  use  of  this  table. 


Acidity 
of  Pulp 

Grams  Lime 
to  be  Added 

Weight  to 
be  Subtracted 

Acidity 
of  Pulp 

Grams  Lime 
to  be  Added 

Weight  to 
be  Subtracted 

.100 

.0100 

.0068 

.600 

.0600 

.0407 

.110 

.0110 

.0075 

.610 

.0610 

.0414 

.120 

.0120 

.0081 

.620 

.0620 

.0420 

.130 

.0130 

.0088 

.630 

.0630 

.0427 

.140 

.0140 

.0095 

.640 

.0640 

.0434 

.150 

.0150 

.0102 

.650 

.0650 

.0441 

•  .160 

.0160 

.0109 

.660 

.0660 

.0448 

.170 

.0170 

.0116 

.670 

.0670 

.0454 

.180 

.0180 

.0122 

.680 

.0680 

.0461 

.190 

.0190 

.0129 

.690 

.0690 

.0468 

.200 

.0200 

.0136 

.700 

.0700 

.0475 

.210 

.0210 

.0143 

.710 

.0710 

.0482 

.220 

.0220 

..0149 

.720 

.0720 

.0488 

.230 

.0230 

.0156 

.730 

.0730 

.0495 

.240 

.0240 

.0162 

.740 

.0740 

.0502 

.250 

.0250 

.0169 

.750 

.0750 

.0509 

.260 

.0260 

.0176 

.760 

.0760 

.0516 

.270 

.0270 

.0183 

.770 

.0770 

.0522 

.280 

.0280 

.0190 

.780 

.0780 

.052.9 

.290 

.0290 

.0196 

.790 

.0790 

.0536 

a 

.300 

.0300 

.0203 

.800 

.0800 

.0543 

.310 

.0310 

.0210 

.810 

.0810 

.0550 

.320 

.0320 

.0217 

.820 

.0820 

.0557 

.330 

.0330 

.0224 

.830 

.0830 

.0564 

.340 

.0340 

.0230 

.840 

.0840 

.0571 

.350 

.0350 

.0237 

.850 

.0850 

.0578 

.360 

.0360 

.0244 

.860 

.0860 

.0585 

.370 

.0370 

.0251 

.870 

.0870 

.0592 

.380 

.0380 

.0258 

.880 

.0880 

.0598 

.390 

.0390 

.0204 

.890 

.0890 

.0605 

.400 

.0400 

.0271 

.900 

.0900 

.0612 

.410 

.0410 

.0278 

.910 

.0910 

.0619 

.420 

.0420 

.0285 

.920 

.0920 

.0626 

.430 

.0430 

.0291 

.930 

.0930 

.0632 

.440 

.0440 

.0298 

.940 

.0940 

.0639 

.450 

.0450 

.0305 

.950 

.0950 

.0646 

.460 

.0460 

.0312 

.960 

.0960 

.0653 

.470 

.0470 

.0319 

.970 

.0970 

.0660 

.480 

."0480 

.0325 

.980 

.0980 

.0666 

.490 

.0490 

.0332 

.990 

.0990 

.0673 

.500 

.0500 

.0339 

1.000 

.1000 

.0680 

.510 

.0510 

.0346 

1.010 

.1010 

.0687 

.520 

.0520 

.0353 

1.020 

.1020 

.0694 

.530 

.05'0 

.0359 

1.030 

.1030 

.0700 

.540 

.0540 

.0366 

1.040 

.1040 

.0707 

.550 

.0550 

.0373 

1.050 

.1050 

.0714 

.560 

.0560 

.0380 

1.060 

.1060 

.0721 

.570 

.0570 

.0387 

1.070 

.1070 

.0728 

.580 

.0580 

.0393 

1.080 

.1080 

.0734 

.590 

.0590 

.0400 

1.090 

.1090 

07-41 

XXVII.       TABLES 


229 


TABLE  17 
B.  T.  U.  LOST  IN  DRY  FLUE  GAS  PER  POUND  OF  COAL  CONTAINING  57%  CARBON 

Based  on  percentage  of  CO?  in  the  flue  gas,  temperature,  °F.,  of  flue  gas  (T),  and  tempera- 
ture, °F.,  of  boiler  room  (t). 


%co, 

T—  t 

250 

255 

260 

265 

270 

275 

280 

285 

290 

295 

6.0 

1401 

1429 

1457 

1485 

1513 

1541 

1569 

1597 

1625 

1653 

6.1 

1379 

1406 

1434 

1462 

1489 

1517 

1544 

1572 

1599 

1627 

6.2 

1357 

1384 

1411 

1438 

1466 

1493 

1520 

1547 

1574 

1601 

6.3 

1336 

1363 

1389 

1416 

1443 

1470 

1496 

1523 

1550 

1577 

6.4 

1316 

1342 

1369 

1395 

1421 

1448 

1474 

1500 

1527 

1553 

6.5 

1296 

1322 

1348 

1374 

1400 

1426 

1452 

1478 

U03 

1529 

6.6 

1277 

1303 

1328 

1354 

1379 

1405 

1430 

1456 

1481 

1507 

6.7 

1259 

1284 

1309 

1335 

1360 

1385 

1410 

1435 

1460 

1486 

6.8 

1241 

1266 

1291 

1315 

1340 

1365 

1390 

1415  . 

1439 

1464 

6.9 

1223 

1247 

1272 

1296 

1321 

1345 

1370 

1394 

1419 

1443 

7.0 

1206 

1230 

1254 

1278 

1302 

1326 

1350 

1375 

1399 

1423 

7.1 

1189 

1213 

1237 

1261 

1285 

1308 

1332 

1356 

1380 

1404 

7.2 

1173 

1197 

1220 

1244 

1267 

1291 

1314 

1338 

1362 

1386 

7.3 

1158 

1181 

1204 

1227 

1250 

1273 

1297 

1320 

1343 

1366 

7.4 

1143 

1165 

1188 

1211 

1234 

1257 

1280 

1302 

1325 

1348 

7.5 

1128 

1150 

1173 

1195 

1218 

1241 

1263 

1286 

1308 

1331 

7.6 

1114 

1136 

1158 

1180 

1203 

1225 

1247 

1269 

1292 

1314 

7.7 

1100 

1121 

1143 

1165 

1187 

1209 

1231 

1253 

1275 

1297 

7.8 

1086 

1108 

1129 

1151 

1173 

1194 

1216 

1238 

1260 

1281 

7.9 

1073 

1094 

1115 

1137 

1158 

1180 

1201 

1223 

1244 

1266  .- 

8.0 

1060 

1081 

1102 

1123 

1144 

1165 

1187 

1208 

1229 

1250 

8.1 

1047 

1068 

1089 

1110 

1131 

1152 

1172 

1193 

1214 

1235, 

8.2 

1034 

1055 

1076 

1097 

1117 

1138 

1159 

1179 

1200 

1221 

8.3 

1022 

1043 

1063 

1084 

1104 

1125 

1145 

1166 

1186 

1206  , 

8.4  :. 

M'- 

1011 

1031 

1051 

1071 

1092 

1112 

1132 

1152 

1172 

1193 

8.5 

1001 

1021 

1041 

1061 

1081 

1101 

1121 

1141 

1161 

1181 

8.6 

988 

1008 

1027 

1047 

1067 

1087 

1107 

1126 

1146 

1166 

8.7 

977 

997 

1016 

1036 

1055 

1075 

1094 

1114 

1133 

1153 

8.8 

966 

986 

1005 

1024 

1044 

1063 

1082 

1102 

1121 

1140 

8.9 

956 

975 

994 

1013 

1032 

1051 

1070 

1090 

1109 

1128 

9.0 

946 

965 

984 

1003 

1022 

1041 

1059 

1078 

1097 

1116 

9.1 

936 

955 

973 

992 

1011 

1030 

1048 

1067 

1086 

1104 

9.2 

926 

945 

963 

982 

1000 

1019 

1037 

1056 

1074 

1093 

93 

918 

936 

955 

973 

991 

1010 

1028 

1047 

1065 

1083 

9.4 

908 

926 

944 

962 

981 

999 

1017 

1035 

1053 

1071 

9.5 

898 

915 

933 

951 

969 

987 

1005 

1023 

1041 

1059 

9.6 

889 

906 

924 

942 

960 

977 

995 

1013 

1031 

1048 

9.7 

880 

897 

915 

932 

950 

968 

985 

1003 

1020 

1038 

9.8 

S71 

889 

906 

924 

941 

958 

976 

993 

1011 

1028 

9.9 

863 

880 

897 

915 

932 

949 

966 

984 

1001 

1018 

10  0 

854 

871 

888 

905 

922 

939 

956 

974 

991 

1001 

10.1 

846 

863 

880 

897 

914 

931 

948 

965 

981 

99S 

10.2 

838 

855 

872 

888 

905 

922 

939 

955 

972 

989 

10.3 

831 

848 

864 

881 

897 

914 

931 

947 

964 

980 

10.4 

823 

839 

856 

872 

889 

905 

922 

938 

955 

971 

230 


METHODS  OP  ANALYSIS 
TABLE  17— Continued 


%C02 

T—  t 

300 

305 

310 

315 

320 

325 

330 

335 

340 

345 

6.0 

1681 

1709 

1737 

1765 

1793 

1821 

1849 

1877 

1905 

1933 

6.1 

1655 

1682 

1710 

1737 

1764 

1793 

1820 

1847 

1875 

1903 

6.2 

1628 

1655 

1683 

1710 

1737 

1764 

1791 

1818 

1846 

1873 

6.3 

1603 

1630 

1657 

1683 

1710 

1737 

1764 

1790 

1817 

1844 

6.4 

1579 

1606 

1632 

1658 

1684 

1711 

1737 

1763 

1790 

1816 

6.5 

1555 

1581 

1607 

1633 

1659 

1685 

1711 

1737 

1763 

1789 

6.6 

1532 

1558 

1583 

1609 

1635 

1660 

1686 

1711 

1737 

1762 

6.7 

1511 

1536 

1561 

1586 

1611 

1637 

1662 

1687 

1712 

1737 

6.8 

1489 

1514 

1539 

1564 

1588 

1613 

1638 

1663 

1688 

1712 

6.9 

1468 

1492 

1517 

1541 

1565 

1590 

1614 

1639 

1663 

1688 

7.0 

1447 

1471 

1495 

1519 

1543 

1567 

1591 

1616 

1640 

1664 

7.1 

1427 

1451 

1475 

1499 

1523 

1546 

1570 

1594 

1618 

1641 

7.2 

1409 

1432 

1455 

1478 

1502 

1525 

1549 

1572 

1596 

1619 

7.3 

1389 

1412 

1435 

1458 

1482 

1505 

1528 

1551 

1574 

1598 

7.4 

1371 

1394 

1417 

1440 

1462 

1485 

1508 

1531 

1554 

1577 

7.5 

1353 

1376 

1398 

1421 

1444 

1466 

1489 

1511 

1534 

1556 

7.6 

1336 

1358 

1381 

1403 

1425 

1448 

1470 

1492 

1514 

1537 

7.7 

1319 

1341 

1363 

1385 

1407 

1429 

1451 

1473 

1495 

1517 

7.8 

1303 

1325 

1347 

1368 

1390 

1412 

1433 

1455 

1477 

1499 

7.9 

1287 

1308 

1330 

1351 

1373 

1394 

1416 

1437 

1459 

1480 

8.0 

1272 

1293 

1314 

1335 

1356 

1378 

1399 

1420 

1441 

1462 

8.1 

1256 

1277 

1298 

1319 

1340 

1361 

1382 

1403 

1424 

1445 

8.2 

1241 

1262 

1283 

1303 

1324 

1345 

1366 

1386 

1407 

1428 

8.3 

1227 

1247 

'  1268 

1288 

1309 

1329 

1350 

1370 

1391 

1411 

8.4 

1213 

1233 

1253 

1273 

1294 

1314 

1334 

1354 

1374 

1395 

8.5 

1201 

1221 

1241 

1261 

1281 

1301 

1321 

1341 

1361 

1381 

8.6 

1186 

1205 

1225 

1245 

1265 

1284 

1304 

1324 

1344 

1363 

8.7 

1172 

1192 

1211 

1231 

1251 

1270 

1290 

1309 

1329 

1348 

8.8 

1160 

1179 

1198 

1218 

1237 

1256 

1275 

1295 

1314 

1334 

8.9 

1147 

1166 

1185 

1204 

1223 

1242 

1262 

1281 

1300 

1319 

9.0 

1135 

1154 

1173 

1192 

1211 

1230 

1249 

1267 

1286 

1305 

9.1 

1123 

1142 

1161 

1179 

1198 

1217 

1235 

1254 

1273 

1291 

9.2 

1111 

1130 

1148 

1167 

1185 

1204 

1222 

1241 

1259 

1278 

9.3 

1102 

1120 

1138 

1157 

1175 

1194 

1212 

1230 

1249 

1267 

9.4 

1089 

1108 

1126 

1144 

1162 

1180 

1198 

1216 

1235 

1253 

9.5 

1077 

1095 

1113 

1131 

1149 

1167 

1185 

1203 

1221 

1239 

9.6 

1066 

1083 

1102 

1120 

1137 

1155 

1173 

1191 

1208 

1226 

9.7 

1055 

1073 

1090 

1108 

1125 

1143 

1160 

1178 

1196 

1213 

9.8 

1045 

1063 

1080 

1098 

1115 

1133 

1150 

1168 

1185 

1202 

9.9 

1035 

1053 

1070 

1087 

1104 

1122 

1139 

1156 

1173 

1191 

10.0 

1025 

1042 

1059 

1076 

1093 

1110 

1127 

1144 

1161 

1179 

10.1 

1015 

1032 

1049 

1066 

1083 

1100 

1117 

1134 

1151 

1168 

10.2 

1006 

1022 

1039 

1056 

1073 

1089 

1106 

1123 

1140 

1156 

10.3 

997 

1014 

1030 

1047 

1064 

1080 

1097 

1113 

1130 

1147 

10.4 

988 

1004 

1021 

1037 

1053 

1070 

1086 

1103 

1119 

1136 

XXVII.      TABLES 
TABLE  17— Continued 


231 


%co, 

T—  t 

350 

355 

360 

365 

370 

375 

380 

385 

390 

395 

6.0 

1961 

1989 

2107 

2045 

2073 

2102 

2136 

2158 

2186 

2214 

6.1 

1931 

1958 

1986 

2013 

2041 

2068 

2096 

2124 

2151 

2179 

6.2 

1900 

1927 

1954 

1981  • 

2008 

2036 

2063 

2089 

2117 

2144 

6.3 

1871 

1897 

1924 

1951 

1978 

2004 

2031 

2058 

2084 

2111 

6.4 

1842 

1869 

1895 

1921 

1948 

1974 

2000 

2027 

2053 

2079 

6.5 

1815 

1841 

1866 

1892 

1918 

1944 

1970 

1996 

2022 

2048 

0.6 

1788 

1814 

1839 

1865 

1890 

1916 

1941 

1967 

1992 

2018 

6.7 

1762 

1788 

1813 

1838 

1863 

1888 

1913 

1939 

1964 

1989 

6.8 

1737 

1762 

1787 

1812 

1836 

1861 

1886 

1911 

1936 

1960 

6.9 

1712 

1737 

1761 

1786 

1810 

1835 

1859 

1883 

1908 

1932 

7.0 

1688 

1712 

1736 

1760 

1785 

1809 

1833 

1857 

1881 

1905 

71 

1665 

1689 

1713 

1737 

1760 

1784 

1808 

1832 

1855 

:879 

7.2 

1643 

1666 

1690 

1713 

1737 

1760 

1784 

1807 

1831 

1854 

7.3 

1621 

1644 

1667 

1690 

1713 

1737 

1760 

1783 

1806 

1829 

7.4 

1600 

1622 

1645 

1668 

1691 

1714 

1737 

1759 

1782 

1805 

7.5 

1579 

1602 

1624 

1647 

1669 

1692 

1714 

1737 

1759 

1782 

7.6 

1559 

1581 

1603 

1626 

1648 

1670 

1692 

1715 

1737 

1759 

7.7 

1539 

1561 

1583 

1605 

1627 

1649 

1671 

1693 

1715 

1737 

7.8 

1520 

1542 

1564 

1585 

1607 

1629 

1651 

1672 

1694 

1716 

7.9 

1502 

1523 

1544 

1566 

1587 

1609 

1630 

1652 

1673 

1695 

8.0 

1483 

1505 

1526 

1547 

1568 

1589 

1610 

1632 

1653 

1674 

81 

1466 

1487 

1507 

1528 

1549 

1570 

1591 

1612 

1633 

1654 

8.2 

1448 

1469 

1490 

1510 

1531 

1552 

1572 

1593 

1614 

1634 

8.3 

1431 

1452 

1472 

1493 

1513 

1534 

1554 

1575 

1595 

1615 

8.4 

1415 

1435 

1455 

1476 

1496 

1516 

1536 

1556 

1577 

1597 

8.5 

1401 

1421 

1441 

1461 

1481 

1501 

1521 

1541 

1561 

1581 

8.6 

1383 

1403 

1423 

1442 

1462 

1482 

1502 

1521 

1541 

1561 

8.7 

1368 

1387 

1407 

1426 

1446 

1466 

1485 

1505 

1524 

1544 

8.8 

1353 

1372 

1392 

1411 

1431 

1450 

1469 

1488 

1508 

1527 

8.9 

1338 

1357 

1376 

1395 

1414 

1434 

1456 

1472 

1490 

1510 

9.0 

1324 

1343 

1362 

1381 

1400 

1419 

1438 

1457 

1475 

1494 

9.1 

1310 

1329 

1348 

1366 

1385 

1404 

1422 

1441 

1460 

1479 

9.2 

1296 

1315 

1333 

1352 

1370 

1389 

1408 

1426 

1445 

1463 

9.3 

1285 

1304 

1322 

1341 

1359 

1377 

1396 

1414 

1432 

1451 

9.4 

1271 

1289 

1307 

1325 

1343 

1362 

1380 

1398 

1416 

1434 

9.5 

1257 

1274 

1291 

1310 

1328 

1346 

1364 

1382 

1400 

1418 

9.6 

1  24  J 

1262 

1279 

1297 

1315 

1333 

1351 

1368 

1386 

1404 

9.7 

1231 

1248 

1264 

1282 

1299 

1317 

1334 

1352 

1369 

1387 

9.8 

1220 

1237 

1255 

1272 

1289 

1307 

1324 

1342 

1359 

1377 

9.9 

1208 

1225 

1242 

1260 

1277 

1294 

1311 

1329 

1346 

1363 

10.0 

1196 

1213 

1230 

1247 

1264 

1281 

1298 

1315 

1332 

1349 

10.1 

1185 

1202 

1218 

1235 

1252 

1269 

1286 

1303 

1320 

1337 

10  2 

1173 

1190 

1207 

1223 

1240 

1257 

1274 

1291 

1307 

1324 

10  3 

1163 

1180 

1196 

1213 

1230 

1246 

1263 

1279 

1296 

1313 

10  4 

1162 

1169 

1185 

1202 

1218 

1235 

1251 

1267 

1284 

1300 

232 


METHODS  OF  ANALYSIS 
TABLE  17— Continued 


%CO2 

T—  t 

400 

405 

410 

415 

420 

425 

430 

435 

440 

445 

6.0 

2242 

2270 

2298 

2326 

2354 

2382 

2410 

2438 

2466 

2494 

6.1 

2206 

2234 

2262 

2289 

2317 

2344 

2372 

2399 

2427 

2455 

6.2 

2171 

2198 

2225 

2253 

2280 

2307 

2334 

2361 

2383 

2415 

6.3 

2138 

2165 

2191 

2218 

2245 

2272 

2298 

2325 

2352 

2378 

6.4 

2106 

2132 

2158 

2185 

2211 

2237 

2264 

2290 

2316 

2342 

6.5 

2074 

2100 

2126 

2152 

2178 

2204 

2230 

2256 

2281 

2307 

6.6 

2043 

2069 

2094 

2120 

2146 

2171 

2197 

2222 

2248 

2273 

6.7 

2014 

2039 

2064 

2090 

2115 

2140 

2165 

2190 

2215 

2241 

6.8 

1985 

2010 

2035 

2060 

2085 

2109 

2134 

2159 

2184 

2209 

6.9 

1957 

1981 

2005 

2030 

2055 

2079 

2104 

2128 

2152 

2177 

7.0 

1929 

1953 

1977 

2002 

2026 

2050 

2074 

2098 

2122 

2146 

7.1 

1903 

1927 

1951 

1974 

1998 

2022 

2046 

2069 

2093 

2117 

7.2 

1877 

1901 

1924 

1948 

1971 

1995 

2018 

2042 

2065 

2089 

7.3 

1852 

1875 

1899 

1922 

1945 

1968 

1991 

2014 

2038 

2061 

7.4 

1828 

1851 

1874 

1897 

1919 

1942 

1965 

1988 

2011 

2034 

7.5 

1805 

1827 

1850 

1872 

1895 

1917 

1940 

1962 

1985 

2068 

7.6 

1782 

1804 

1826 

1848 

1871 

1893 

1915 

1937 

1960 

1982 

7.7 

1759 

1781 

1803 

1825 

1847 

1869 

1891 

1913 

1935 

1957 

7.8 

1737 

1759 

1781 

1803 

1824 

1846 

1868 

1890 

1911 

1933 

7.9 

1716 

1737 

1759 

1780 

1802 

1823 

1845 

1866 

1888 

1909 

8.0 

1695 

1716 

1738 

1759 

1780 

1801 

1822 

1844 

1865 

1886 

8.1 

1675 

1696 

1717 

1738 

1759 

1780 

1801 

1821 

1842 

1863 

8.2 

1655 

1676 

1697 

1717 

1738 

1759 

1779 

1800 

1821 

1841 

8.3 

1636 

1656 

1677 

1697 

1718 

1738 

1759 

1779 

1799 

1820 

8.4 

1617 

1637 

1657 

1678 

1698 

1718 

1738 

1758 

1779 

1799 

8.5 

1601 

1621 

1641 

1661 

1681 

1701 

1721 

1741 

1761 

1781 

8.6 

1581 

1601 

1620 

1640 

1660 

1680 

1699 

1719 

1739 

1759 

8.7 

1563 

1583 

1602 

1622 

1641 

1661 

1680 

1700 

1720 

1739 

8.8 

1546 

1566 

1585 

1604 

1624 

1643 

1662 

1682 

1701 

1720 

8.9 

1529 

1548 

1567 

1586 

1605 

1625 

1644 

1663 

1682 

1701 

9.0 

1513 

1532 

1551 

1570 

1589 

1608 

1627 

1646 

1665 

1683 

9.1 

1497 

1516 

1535 

1553 

1572 

1591 

1610 

1628 

1647 

1666 

9.2 

1482 

1500 

1519 

1537 

1556 

1574 

1593 

1611 

1630 

1648 

9.3 

1469 

1487 

1506 

1524 

1543 

1561 

1579 

1598 

1616 

1634 

9.4 

1452 

1470 

1488 

1507 

1525 

1543 

1561 

1579 

1597 

1615 

9.5 

1436 

1454 

1472 

1490 

1508 

1526 

1544 

1562 

1580 

1598 

9.6 

1422 

1439 

1457 

1475 

1493 

1510 

1528 

1546 

1564 

1582 

9.7 

1405 

1422 

1440 

1457 

1475 

1492 

1510 

1528 

1545 

1563 

9.8 

1394 

1411 

1429 

1446 

1464 

1481 

1499 

1516 

1533 

1551 

9.9 

1380 

1398 

1415 

1432 

1449 

1467 

1484 

1501 

1518 

1536 

10.0 

1366 

1383 

1401 

1418 

1435 

1452 

1469 

1486 

1503 

1520 

10.1 

1354 

1371 

1388 

1405 

1422 

1439 

1455 

1472 

1489 

1506 

10.2 

1341 

1358 

1374 

1391 

1408 

1425 

1441 

1458 

1475 

1492 

10.3 

1329 

1346 

1363 

1379 

1396 

1412 

1429 

1446 

1462 

1479 

10.4 

1317 

1333 

1350 

1366 

1383 

1399 

1416 

1432 

1448 

1465 

XXVII.      TABLES 
TABLE  17— Continued 


233 


•%  co, 

T—  t 

450 

455 

460 

465 

470 

475 

480 

485 

490 

495 

6.0 

2522 

2550 

2578 

2606 

2634 

2662 

2690 

2718 

2746 

2774 

61 

2482 

2510 

2537 

2565 

2593 

2620 

2648 

2675 

2703 

2730 

6.2 

2443 

2470 

2497 

2524 

2551 

2578 

2605 

2633 

2660 

2687 

6.3 

2305 

2432 

2459 

2485 

2512 

2539 

2566 

2592 

2619 

2646 

6.4 

2369 

2395 

2421 

2448 

2474 

2500 

2527 

2553 

2579 

2606 

6.5 

2333 

2357 

2385 

2411 

2437 

2463 

2489 

2515 

2541 

2567 

6.6 

2299 

2324 

2356 

2375 

2401 

2427 

2452 

2478 

2508 

2529 

6.7 

2266 

2291 

2316 

2341 

2366 

2392 

2417 

2442 

2467 

2492 

6.8 

2233 

2258 

2283 

2308 

2333 

2357 

2382 

2407 

2432 

2457 

6.9 

2201 

2226 

2250 

2275 

2299 

2324 

2348 

2373 

2397 

2422 

7.0 

2170 

2194 

2219 

2243 

2267 

2291 

2315 

2339 

2363 

2387 

7.1 

2141 

2165 

2188 

2212 

2236 

22CO 

2284 

2307 

2331 

2355 

7.2 

2112 

2136 

2159 

2183 

2206 

2229 

2253 

2276 

2300 

2323 

7.3 

2084 

2107 

2130 

2153 

2176 

2200 

2223 

2246 

2269 

2292 

7.4 

2057 

2079 

2102 

2125 

2148 

2171 

2194 

2216 

2239 

2262 

7.5 

2030 

2053 

2075 

2098 

2120 

2143 

2165 

2188 

2211 

2233 

7.6 

2004 

2027 

2049 

2071 

2093 

2116 

2138 

2160 

2182 

2205 

7.7 

1979 

2001 

2023 

2045 

2067 

2089 

2111 

2133 

2155 

2177 

7.8 

1955 

1976 

1998 

2020 

2042 

2063 

2085 

2107 

2128 

2150 

7.9 

1931 

1952 

1973 

1995 

2016 

2038 

2059 

2081 

2102 

2124 

8.0 

1907 

1928 

1950 

1971 

1992 

2013 

2034 

2055 

2077 

2098 

8.1 

1884 

1905 

1926 

1947 

1968 

1989 

2010 

2031 

2052 

2072 

8.2 

1862 

1883 

1903 

1924 

1945 

1966 

1986 

2007 

2028 

2048 

8.3 

1840 

1861 

1881 

1901 

1922 

1943 

1963 

1984 

2004 

2024 

8.4 

1819 

1839 

1860 

1880 

1900 

1920 

1940 

1961 

1981 

2001 

8.5 

1801 

1821 

1841 

1861 

1881 

1901 

1921 

1941 

1961 

1981 

8.6 

1778 

1798 

1818 

1838 

1857 

1877 

1897 

1917 

1936 

1956 

8.7 

1759 

1778 

1797 

1817 

1837 

1856 

1876 

1895 

1915 

1934 

8.8 

1740 

1759 

1778 

1798 

1817 

1836 

1856 

1875 

1894 

1914 

8.9 

1720 

1739 

1758 

1777 

1797 

1816 

1835 

1854 

1873 

1892 

9.0 

1702 

1721 

1740 

1759 

1778 

1797 

1816 

1835 

1854 

1873 

91 

1684 

1703 

1722 

1741 

1759 

1778 

1797 

1815 

1834 

1853 

9.2 

1667 

1685 

1704 

1722 

1741 

1759 

1778 

1796 

1815 

1833 

9.3 

1653 

1671 

1690 

1708 

1726 

1745 

1763 

1781 

1800 

1818 

9.4 

1634 

1652 

1670 

1688 

1707 

1725 

1743 

1761 

1779 

1797 

9.5 

1616 

1633 

1651 

1669 

1687 

1705 

1723 

1741 

1759 

1777 

9.6 

1599 

1617 

1635 

1653 

1670 

1688 

1706 

1724 

1741 

1759 

9.7 

1580 

1598 

1615 

1633 

1650 

1668 

1685 

1703 

1720 

1738 

9.8 

1568 

1586 

1603 

1621 

1638 

1655 

1673 

1690 

1708 

1725 

9.9 

1553 

1570 

1587 

1605 

1622 

1639 

1657 

1674 

1691 

1708 

10.0 

1537 

1554 

1571 

1588 

1606 

1623 

1640 

1657 

1674 

1691 

10.1 

1523 

1540 

1557 

1574 

1591 

1608 

1625 

1642 

1659 

1676 

10  2 

1508 

1525 

1542 

1559 

1575 

1592 

1609 

1626 

1642 

1659 

10  3 

1495 

1512 

1529 

1545 

1562 

1578 

1595 

1612 

1628 

1645 

10.4 

1481 

1498 

1514 

1531 

1547 

1564 

1580 

1597 

1613 

1630 

234 


METHODS  OP   ANALYSIS 
TABLE  17— Continued 


T—  t 

07  ro. 

/O  ^^2 

500 

505 

510 

515 

520 

525 

530 

535 

540 

545 

550 

6.0 

2803 

2830 

2858 

2886 

2914 

2942 

2970 

2998 

3026 

3054 

3082 

6.1 

2758 

2786 

2813 

2841 

2868 

2896 

2923 

2651 

2979 

3006 

3034 

6.2 

2714 

2741 

2768 

2795 

2823 

2850 

2877 

2904 

2931 

2958 

2985 

6.3 

2673 

2699 

2726 

2753 

2779 

2806 

2833 

2860 

2886 

2913 

2940 

6.4 

2632 

2658 

2685 

2711 

2737 

2764 

2790 

2816 

2843 

2869 

2891 

6.5 

2593 

2618 

2644 

2670 

2696 

2722 

2748 

2774 

2800 

2825 

2850 

6.6 

2554 

2580 

2605 

2631 

2656 

2682 

2707 

2733 

2759 

2784 

2810 

6.7 

2517 

2543 

2568 

2593 

2618 

2643 

2669 

2694 

2719 

2744 

2769 

8.8 

2482 

2506 

2531 

2556 

2581 

2606 

2630 

2655 

2680 

2705 

2730 

6.9 

2446 

2470 

2495 

2519 

2544 

2568 

2593 

2617 

2642 

2666 

2691 

7.0 

2412 

2436 

2460 

2484 

2508 

2532 

2556 

2580 

2604 

2629 

2653 

7.1 

2379 

2403 

2426 

2450 

2474 

2498 

2521 

2545 

2569 

2593 

2617 

7.2 

2347 

2370 

2394 

2417 

2441 

2464 

2488 

2511 

2535 

2558 

2581 

7.3 

2315 

2339 

2362 

2385 

2408 

2431 

2454 

2477 

2501 

2524 

2547 

7.4 

2285 

2208 

2331 

2354 

2376 

2399 

2422 

2445 

2468 

2491 

2514 

7.5 

2256 

2278 

2301 

2324 

2346 

2369 

2391 

2414 

2436 

2459 

2481 

7.6 

2227 

2249 

2271 

2294 

2316 

2338 

2361 

2383 

2405 

2427 

2450 

7.7 

2199 

2221 

2243 

2264 

2287 

2309 

2331 

2353 

2375 

2397 

2419 

7.8 

2172 

2194 

2215 

2237 

2259 

2280 

2302 

2324 

2346 

2367 

2389 

7.9 

2145 

2166 

2188 

2209 

2231 

2252 

2274 

2295 

2317 

2338 

2360 

8.0 

2119 

2140 

2161 

2183 

2204 

2225 

2246 

2267 

2282 

2310 

2331 

8.1 

2094 

2115 

2136 

2156 

2177 

2198 

2119 

2240 

2261 

2282 

2303 

8.2 

2069 

2089 

2110 

2131 

2152 

2172 

2193 

2114 

2234 

2255 

2276 

8.3 

2045 

2065 

2086 

2106 

2127 

2147 

2168 

2188 

2209 

2229 

2249 

8.4 

2021 

2041 

2062 

2082 

2102 

2122 

2142 

2163 

2183 

2203 

2223 

8.5 

2001 

2021 

2041 

2061 

2081 

2101 

2121 

2141 

2161 

2181 

2201 

8.6 

1976 

1996 

2015 

2035 

2055 

2075 

2095 

2114 

2134 

2154 

2174 

8.7 

1953 

1974 

1993 

2013 

2032 

2052 

2071 

2091 

2110 

2130 

2149 

8.8 

1933 

1952 

1972 

1991 

2010 

2030 

2049 

2068 

2088 

2107 

2126 

8.9 

1911 

1930 

1950 

1969 

1988 

2007 

2026 

2045 

2064 

2083 

2103 

9.0 

1892 

1910 

1929 

1948 

1967 

1986 

2005 

2024 

2043 

2081 

2100 

9.1 

1872 

1890 

1909 

1928 

1946 

1965 

1984 

2002 

2021 

2040 

2059 

9.2 

1852 

1871 

1889 

1908 

1926 

1945 

1963 

1982 

2000 

2019 

2037 

9.3 

1837 

1855 

1873 

1892 

1910 

1928 

1947 

1965 

1983 

2002 

2020 

9.4 

1816 

1834 

1852 

1870 

1888 

1906 

1924 

1942 

1961 

1979 

1997 

9.5 

1795 

1813 

1831 

1849 

1867 

1885 

1903 

1921 

1939 

1957 

1974 

9.6 

1777 

1795 

1813 

1830 

1848 

1866 

1884 

1901 

1919 

1937 

1955 

9.7 

1756 

1773 

1791 

1808 

1826 

1843 

1861 

1878 

1896 

1913 

1931 

9.8 

1743 

1760 

1777 

1795 

1812 

1830 

1847 

1864 

1882 

1899 

1917 

9.9 

1726 

1743 

1760 

1777 

1795 

1812 

1821 

1846 

1863 

1880 

1898 

10.0 

1708 

1725 

1742 

1759 

1776 

1793 

1810 

1828 

1845 

1862 

1879 

10.1 

1693 

1709 

1726 

1743 

1760 

1777 

1794 

1811 

1828 

1845 

1862 

10.2 

1676 

1693 

1710 

1726 

1743 

1760 

1777 

1793 

1810 

1827 

1844 

10.3 

1662 

1678 

1695 

1711 

1728 

1745 

1761 

1778 

1795 

1811 

1828 

10.4 

1646 

1662 

1679 

1695 

1712 

1728 

1745 

1761 

1778 

1794 

1810 

XXVII.       TABLES 


235 


TABLE  17— Continued 


%co, 

T—  t 

250 

255 

260 

265 

270 

275 

280 

285 

290 

295 

10.5 

815 

832 

848 

864 

881 

891 

913 

930 

946 

962 

10.6 

808 

824 

840 

856 

873 

889 

905 

921 

937 

953 

10.7 

801 

817 

833 

849 

865 

881 

897 

913 

929 

945 

10.8 

794 

810 

826 

842 

857 

873 

889 

905 

921 

937 

10.9 

787 

803 

818 

834 

850 

866 

881 

897 

913 

929 

11.0 

780 

796 

811 

827 

842 

858 

874 

889 

905 

920 

11.1 

773 

788 

804 

819 

835 

859 

866 

881 

897 

912 

11.2 

766 

782 

797 

812 

828 

843 

858 

874 

889 

904 

11.3 

760 

775 

790 

806 

821 

836 

851 

866 

882 

897 

11.4 

754 

709 

785 

803 

815 

830 

846 

861 

876 

891 

11.5 

748 

763 

778 

793 

808 

823 

838 

853 

868 

883 

11  6 

742 

757 

772 

787 

801 

816 

831 

846 

861 

876 

11.7 

736 

751 

765 

780 

795 

810 

824 

839 

854 

868 

11.8 

730 

745 

759 

774 

788 

803 

818 

832 

847 

861 

11.9 

724 

738 

753 

767 

782 

796 

810 

825 

839 

854 

12.0 

719 

733 

748 

762 

776 

791 

805 

820 

834 

848 

12.1 

713 

727 

742 

756 

770 

784 

799 

813 

827 

841 

12.2 

707 

721 

735 

749 

764 

778 

792 

806 

820 

834 

12.3 

702 

716 

730 

744 

758 

772 

786 

800 

814 

828 

12.4 

696 

710 

724 

738 

757 

766 

780 

794 

807 

821 

12.5 

691 

705 

719 

732 

746 

760 

774 

788 

802 

815 

12.6 

686 

700 

713 

727 

741 

755 

768 

782 

796 

809 

12.7 

680 

694 

707 

721 

734 

748 

762 

775 

789 

802 

12.8 

675 

689 

702 

716 

729 

743 

756 

770 

783 

797 

12.9 

670 

683 

697 

710 

724 

737 

750 

764 

777 

791 

13.0 

665 

678 

692 

705 

718 

732 

745 

758 

771 

786 

13.1 

660 

673 

686 

700 

713 

726 

739 

752 

766 

779 

13.2 

656 

669 

682 

695 

708 

722 

735 

748 

761 

774 

13.3 

651 

664 

677 

690 

703 

716 

729 

742 

755 

768 

13.4 

646 

659 

672 

685 

698 

711 

724 

737 

749 

762 

13.5 

642 

655 

668 

681 

693 

706 

719 

732 

745 

758 

13.6 

637 

650 

663 

675 

688 

701 

714 

726 

739 

752 

13.7 

633 

646 

658 

671 

684 

696 

709 

722 

734 

747 

13.8 

628 

641 

653 

666 

678 

691 

703 

716 

729 

741 

13.9 

624 

636 

649 

661 

674 

686 

699 

711 

724 

736 

14.0 

620 

632 

645 

657 

670 

682 

694 

707 

719 

732 

14.1 

616 

628 

641 

653 

665 

678 

690 

702 

715 

727 

14.2 

612 

624 

636 

649 

661 

673 

685 

698 

710 

722 

14.3 

608 

620 

632 

644 

657 

669 

681 

693 

705 

717 

14.4 

604 

616 

628 

640 

652 

664 

676 

689 

701 

713 

14.5 

600 

612 

624 

636 

648 

660 

672 

684 

696 

708 

14.6 

596 

608 

620 

632 

644 

656 

668 

679 

691 

703 

14.7 

592 

604 

616 

628 

639 

651 

663 

675 

687 

699 

14.8 

588 

600 

612 

623 

635 

647 

659 

670 

682 

694 

14.9 

585 

597 

508 

620 

632 

643 

655 

667 

679 

690 

1.5.0 

581 

593 

604 

616 

627 

639 

651 

662 

674 

686 

236 


METHODS  OF   ANALYSIS 


TABLE  17— Continued 


%CO2 

T-t 

300 

305 

310 

315 

320 

325 

330 

335 

340 

345 

10.5 

979 

995 

1011 

1027 

1044 

1060 

1076 

1092 

1109 

1125 

10.6 

970 

986 

1002 

1018 

1034 

1050 

1067 

1083 

1099 

1115 

10.7 

961 

977 

993 

1009 

1025 

1041 

1057 

1073 

1089 

1105 

10.8 

953 

969 

984 

1000 

1016 

1032 

1048 

1064 

1080 

1095 

10.9 

944 

960 

976 

991 

1007 

1023 

1039 

1054 

1070 

1086 

11.0 

936 

952 

967 

983 

998 

1014 

1030 

1045 

1061 

1076 

11.1 

928 

943 

959 

974 

989 

1005 

1020 

1036 

1051 

1067 

11.2 

920 

935 

950 

966 

981 

996 

1012 

1027 

1042 

1058 

11.3 

912 

927 

942 

958 

973 

988 

1003 

1018 

1034 

1049 

11.4 

906 

921 

936 

951 

966 

981 

996 

1012 

1027 

1042 

11.5 

898 

913 

928 

943 

958 

973 

988 

1002 

1017 

1032 

11.6 

890 

905 

920 

935 

950 

965 

979 

994 

1009 

1024 

11.7 

883 

898 

913 

927 

942 

957 

972 

986 

1001 

1016 

11.8 

876 

891 

905 

920 

935 

949 

964 

978 

993 

1008 

11.9 

868 

882 

897 

911 

926 

940 

954 

969 

983 

998 

12.0 

863 

887 

891 

906 

920 

935 

949 

963 

978 

992 

12.1 

856 

870 

884 

898 

913 

927 

941 

955 

970 

984 

12.2 

849 

863 

877 

891 

905 

919 

933 

948 

962 

976 

12.3 

842 

856 

870 

884 

898 

913 

927 

941 

955 

969 

12.4 

835 

849 

863 

877 

891 

905 

919 

933 

947 

961 

12.5 

829 

843 

857 

871 

884 

898 

912 

926 

940 

954 

12.6 

823 

837 

851 

864 

878 

892 

906 

919 

933 

947 

12.7 

816 

830 

843 

857 

870 

884 

898 

911 

925 

938 

12.8 

810 

824 

837 

851 

864 

878 

891 

905 

918 

932 

12.9 

804 

817 

831 

844 

858 

871 

884 

898 

911 

925 

13.0 

798 

811 

825 

838 

851 

865 

878 

891 

904 

918 

13.1 

792 

805 

819 

832 

845 

858 

871 

885 

898 

911 

13.2 

787 

800 

813 

826 

840 

853 

866 

879 

892 

905 

13.3 

781 

794 

807 

820 

833 

846 

859 

872 

885 

898 

13.4 

775 

.788 

801 

814 

827 

840 

853 

866 

879 

892 

13.5 

770 

783 

796 

809 

822 

835 

847 

860 

873 

886 

13.6 

765 

777 

790 

803 

816 

828 

841 

854 

867 

879 

13.7 

760 

772 

785 

797 

810 

823 

835 

848 

861 

873 

13.8 

754 

766 

779 

791 

804 

817 

829 

842 

854 

867 

13.9 

749 

761 

774 

786 

799 

811 

824 

836 

849 

861 

14.0 

744 

756 

769 

781 

794 

806 

818 

831 

843 

856 

14.1 

739 

752 

764 

776 

788 

801 

813 

825 

838 

850 

14.2 

734 

747 

759 

771 

783 

796 

808 

820 

832 

845 

14.3 

730 

742 

754 

766 

778 

790 

803 

815 

827 

839 

14.4 

725 

737 

749 

761 

773 

785 

797 

.  809 

821 

834 

14.5 

720 

732 

744 

756 

768 

780 

792 

804 

816 

828 

14.6 

715 

727 

739 

751 

763 

775 

787 

799 

811 

822 

14.7 

711 

722 

734 

746 

758 

770 

782 

793 

805 

817 

14.8 

706 

717 

729 

741 

753 

764 

776 

788 

800 

811 

14.9 

702 

714 

725 

737 

749 

760 

772 

784 

795 

807 

15.0 

697 

709 

720 

732 

744 

755 

767 

779 

790 

802 

XXVII.       TABLES 


237 


TABLE  17— Continued 


%co, 

T—  t 

350 

355 

360 

365 

370 

375 

380 

385 

390 

395 

10.5 

1142 

1158 

1174 

1191 

1207 

1223 

1239 

1256 

1272 

1288 

10.6 

1131 

1147 

1164 

1179 

1196 

1212 

1228 

1244 

1260 

1277 

10.7 

1121 

1137 

1153 

1169 

1185 

1202 

1217 

1234 

1249 

1266 

10.8 

1111 

1127 

1143 

1159 

1175 

1191 

1207 

1222 

1238 

1254 

10.9 

1102 

1117 

.1133 

1149 

1165 

1180 

1196 

1212 

1226 

1243 

11.0 

1092 

1108 

1123 

1139 

1154 

1170 

1186 

1201 

1217 

1232 

11.1 

1082 

1098 

1113 

1129 

1144 

1160 

1175 

1190 

1206 

1221 

11.2 

1073 

1088 

1104 

1119 

1134 

1150 

1165 

1180 

1196 

1211 

11.3 

1064 

1079 

1094 

1109 

1125 

1140 

1155 

1170 

1186 

1201 

11.4 

1057 

1072 

1087 

1102 

1117 

1132 

1147 

1162 

1178 

1193 

11.5 

1047 

1062 

1077 

1092  , 

1107 

1122 

1137 

1152 

1167 

1182 

11.6 

1039 

1054 

1068 

1083 

1098 

1113 

1128 

1143 

1158 

1172 

11.7 

1030 

1045 

1060 

1075 

1089 

1104 

1119 

1133 

1148 

1163 

11.8 

1022 

1037 

1051 

1066 

1081 

1095 

1110 

1124 

1139 

1154 

11.9 

1012 

1026 

1041 

1055 

1070 

1084 

1099 

1113 

1127 

1142 

12.0 

1006 

1021 

1035 

1050 

1064 

1078 

1093 

1107 

1121 

1136 

12.1 

998 

1012 

1027 

1041 

1055 

1070 

1084 

1098 

1113 

1127 

12.2 

990 

1004 

1018 

1032 

1047 

1061 

1075 

1089 

1103 

1117 

12.3 

983 

997 

1011 

1025 

1039 

1053 

1067 

1081 

1095 

1109 

12.4 

975 

989 

1002 

1016 

1030 

1044 

1058 

1072 

1086 

1100 

12.5 

967 

981 

995 

1009 

1023 

1037 

1050 

1064 

1078 

1092 

12.6 

960 

974 

988 

1002 

1015 

1029 

1043 

1056 

1070 

1084 

12.7 

952 

966 

979 

993 

1006 

1020 

1034 

1047 

1061 

1074 

12.8 

945 

959 

972 

986 

999 

1013 

1026 

1046 

1053 

1067 

12.9 

938 

951 

965 

978 

992 

1005 

1018 

1032 

1045 

1059 

13.0 

931 

944 

958 

971 

984 

998 

1011 

1024 

1037 

1051 

13.1 

924 

937 

951 

964 

977 

990 

1003 

1017 

1030 

1043 

13.2 

918 

931 

944 

958 

971 

984 

997 

1010 

1023 

1036 

13.3 

911 

924 

937 

950 

963 

977 

990 

1003 

1016 

1029 

13.4 

905 

918 

930 

943 

956 

969 

982 

995 

1008 

1021 

13.5 

899 

912 

924 

937 

950 

963 

976 

989 

1002 

1014 

13.6 

892 

905 

918 

930 

943 

956 

969 

981 

994 

1007 

13.7 

886 

899 

911 

924 

937 

949 

962 

975 

987 

1000 

13.8 

879 

x'.rj 

905  ' 

917 

930 

942 

955 

967 

980 

993 

13.9 

874 

sst) 

899 

911 

924 

936 

949 

961 

974 

986 

14.0 

868 

880 

893 

905 

918 

930 

942 

955 

967 

980 

14  1 

862 

875 

887 

899 

912 

924 

936 

949 

961 

973 

14.2 

857 

869 

881 

894 

906 

918 

930 

942 

955 

967 

14  3 

851 

863 

876 

888 

900 

912 

924 

936 

948 

961 

14.4 

s4C> 

858 

870 

SS'J 

894 

906 

918 

930 

942 

954 

14.5 

840 

852 

864 

876 

sss 

900 

912 

924 

936 

948 

14.6 

834 

846  s 

858 

870 

SS2 

894 

906 

918 

930 

942 

1  1  7 

829 

841 

853 

864 

876 

888 

900 

912 

924 

935 

14.8 

823 

835 

847 

858 

870 

882 

894 

906 

917 

929 

14.9 

819 

830 

842 

854 

866 

877 

889 

901 

912 

924 

15.0 

813 

825 

837 

848 

860 

872 

883 

x'.».-> 

906 

918 

238 


METHODS  OF  ANALYSIS 


TABLE  17— Continued 


%C02 

T—  t 

400 

405 

410 

415 

420 

425 

430 

435 

440 

445 

10.5 

1305 

1321 

1337 

1354 

1370 

1386 

1403 

1419 

1435 

1451 

10.6 

1293 

1309 

1325 

1341 

1357 

1374 

1390 

1406 

1422 

1438 

10.7 

1282 

1298 

1314 

1330 

1346 

1362 

1378 

1394 

1410 

1426 

10.8 

1270 

1286 

1302 

1318 

1334 

1349 

1365 

1381 

1397 

1413 

10.9 

1259 

1275 

1290 

1306 

1322 

1338 

1353  • 

1369 

1385 

1400 

11.0 

1248 

1264 

1279 

1295 

1310 

1326 

1342 

1357 

1373 

1385 

11.1 

1237 

1252 

1268 

1283 

1299 

1314 

1330 

1345 

1360 

1376 

11.2 

1226 

1242 

1257 

1272 

1288 

1303 

1318 

1334 

1349 

1364 

11.3 

1216 

1231 

1246 

1262 

1277 

1292 

1307 

1322 

1338 

1353 

11.4 

1208 

1223 

1238 

1253 

1268 

1283 

1298 

1313 

1328 

1344 

11.5 

1197 

1212 

1227 

1242 

1257 

•1272 

1287 

1302 

1317 

1332 

11.6 

1187 

1202 

1217 

1232 

1247 

1261 

1276 

1291 

1306 

1321 

11.7 

1178 

1192 

1207 

1222 

1236 

1251 

1266 

1281 

1295 

1310 

11.8 

1168 

1183 

1198 

1212 

1228 

1241 

1256 

1271 

1285 

1300 

11.9 

1156 

1171 

1185 

1199 

1214 

1228 

1243 

1257 

1271 

1286 

12.0 

1150 

1164 

1179 

1193 

1208 

1222 

1236 

1251 

1265 

1279 

12.1 

1141 

1155 

1169 

1184 

1198 

1212 

1226 

1241 

1255 

1269 

12.2 

1132 

1146 

1160 

1174 

1188 

1202 

1216 

1231 

1245 

1259 

12.3 

1123 

1137 

1151 

1165 

1179 

1193 

1207 

1221 

1236 

1250 

12.4 

1114 

1128 

1142 

1156 

1170 

1184 

1197 

1211 

1225 

1239 

12.5 

1108 

1119 

1133 

1147 

1161 

1175 

1189 

1202 

1216 

1230 

12.6 

1098 

1111 

1125 

1139 

1152 

1166 

1180 

1194 

1207 

1221 

12.7 

1088 

1102 

1115 

1129 

1142 

1156 

1170 

1183 

1197 

1210 

12.8 

1080 

1094 

1107 

1121 

1134 

1148 

1161 

1175 

1183 

1202 

12.9 

1072 

1085 

1099 

1112 

1126 

1139 

1152 

1166 

1179 

1193 

13.0 

1064 

1077 

1091 

1104 

1117 

1131 

1144 

1157 

1170 

1184 

13.1 

1056 

1070 

1083 

1096 

1109 

1122 

1136 

1149 

1162 

1175 

13.2 

1049 

1062 

1076 

1089 

1102 

1115 

1128 

1141 

1154 

1167 

13.3 

1042 

1055 

1038 

1081 

1094 

1107 

1120 

1133 

1148 

1159 

13.4 

1034 

1047 

1060 

1073 

1086 

1099 

1111 

1124 

1137 

1150 

13.5 

1027 

1040 

1053 

1056 

1079 

1091 

1109 

1117 

1130 

1143 

13.6 

1020 

1032 

1015 

1058 

1071 

1083 

1096 

1109 

1122 

1134 

13.7 

1013 

1025 

1038 

1050 

1063 

1076 

1088 

1101 

1114 

1126 

13.8 

1005 

1018 

1030 

1043 

1055 

1068 

1081 

1093 

1106 

1118 

13.9 

999 

1011 

1023 

1036 

1049 

1061 

1074 

1086 

1099 

1111 

14.0 

992 

1004 

1017 

1029 

1042 

1054 

1066 

1079 

1091 

1104 

14.1 

986 

998 

1010 

1023 

1035 

1047 

1060 

1072 

1084 

1096 

14.2 

979 

991 

1004 

1016 

1028 

1040 

1053 

1065 

1077 

1089 

14.3 

973 

985 

997 

1001 

1029 

1074 

1046 

1058 

1070 

1082 

14.4 

966 

978 

991 

1003 

1015 

1027 

1039 

1051 

1063 

1075 

14.5 

960 

972 

984 

996 

1008 

1020 

1032 

1044 

1056 

1068 

14.6 

954 

966 

977 

989 

1001 

1013 

1025 

1037 

1049 

1061 

14.7 

947 

959 

971 

983 

995 

1007 

1018 

1030 

1042 

1054 

14.8 

941 

953 

964 

976 

988 

1000 

1011 

1023 

1035 

1047 

14.9 

936 

947 

959 

971 

982 

994 

1006 

1018 

1029 

1041 

15.0 

930 

941 

953 

964 

976 

988 

999 

1011 

1023 

1034 

XXVII.       TABLES 


239 


TABLE  17— Continued 


%co, 

T—  t 

450 

455 

460 

465 

470 

475 

480 

485 

490 

495 

10.5 

1468 

1484 

1500 

1517 

1533 

1549 

1566 

1582 

1598 

1615 

10.6 

1454 

1471 

1487 

1503 

1519 

1535 

1551 

1568 

1584 

1600 

10.7 

1442 

1458 

1474 

1490 

1506 

1522 

1538 

1554 

1570 

1586 

10.8 

1429 

L446 

1461 

1476 

1492 

1508 

1524 

1540 

1556 

1572 

10.9 

1416 

1432 

1448 

1463 

1479 

1495 

1511 

1526 

1542 

1558 

11.0 

1404 

1420 

1435 

1451 

1466 

1482 

1498 

1513 

1529 

1544 

11.1 

1391 

1407 

1422 

1438 

1453 

1469 

1484 

1500 

1515 

1531 

11  2 

1380 

1395 

1410 

1426 

1441 

1456 

1472 

1487 

1502 

1518 

11  3 

1369 

1383 

1398 

1414 

1429 

1444 

1459 

1474 

1490 

1505 

11.4 

1359 

1374 

1389 

1404 

1419 

1434 

1449 

1464 

1479 

1494 

11.5 

1347 

1362 

1377 

1392 

1407 

1422 

1437 

1152 

1467 

1482 

11.6 

1336 

1350 

1365 

1380 

1395 

1410 

1425 

1439 

1454 

1469 

11.7 

1325 

1340 

1354 

1369 

1384 

1398 

1413 

1428 

1443 

1457 

11.8 

1314 

1329 

1344 

1358 

1373 

1387 

1402 

1417 

1431 

1446 

11  9 

1300 

1315 

1329 

1343 

1358 

1372 

1387 

1401 

1416 

1430 

12.0 

1294 

1308 

1323 

1337 

1351 

1366 

1380 

1394 

1409 

1423 

12  1 

1283 

1298 

1312 

1326 

1340 

1355 

1369 

1383 

1397 

1412 

12  2 

1273 

1287 

1301 

1315 

1330 

1344 

1358 

1372 

1386 

1400 

12.3 

1264 

1278 

1292 

1306 

1320 

1334 

1348 

1362 

1376 

1390 

12  4 

1253 

1267 

1281 

1295 

1309 

1323 

1337 

1351 

1365 

1379 

12.5 

1244 

1258 

1271 

1285 

1299 

1313 

1327 

1341 

1354 

1368 

12.6 

1235 

1249 

1262 

1276 

1290 

1303 

1317 

1331 

1345 

1358 

12.7 

1224 

1238 

1251 

1265 

1278 

1292 

1306 

1319 

1333 

1346 

12.8 

1215 

1229 

1242 

1256 

1269 

1283 

1296 

1310 

1323 

1337 

12.9 

1206 

1219 

1233 

1246 

1260 

1273 

1286 

1300 

1313 

1327 

13.0 

1197 

1210 

1224 

1237 

1250 

1264 

1277 

12fiO 

1303 

1317 

1  13.1 

1188 

1202 

1215 

1228 

1241 

1254 

1268 

1281 

1294 

1307 

13.2 

1180 

1194 

1207 

1220 

1233 

1246 

1259 

1272 

1285 

1298 

13.3 

1172 

1185 

1198 

1211 

1224 

1237 

1250 

1263 

1276 

1289 

13.4 

1163 

1176 

1189 

1202 

1215 

1228 

1241 

1254 

1267 

1280 

13.5 

1156 

1168 

1181 

1194 

1207 

1220 

1233 

1245 

1258 

1271 

13.6 

1147 

1160 

1173 

1185 

1198 

1211 

1224 

1236 

1249 

1262 

13  7 

1139 

1152 

1164 

1177 

1190 

1202 

1215 

1228 

1240 

1253 

13.8 

1131 

1143 

1156 

1169 

1181 

1194 

1206 

1219 

1231 

1244 

13  9 

1124 

1136 

1149 

1161 

1174 

1186 

1199 

1211 

1224 

1236 

14.0 

1116 

1128 

1141 

1153 

1166 

1178 

1190 

1203 

1215 

1228 

14  1 

1109 

1121 

1133 

1146 

1158 

1170 

1183 

1195 

1207 

1220 

14  2 

1102 

1114 

1126 

1138 

1151 

1163 

1175 

1187 

1200 

1212 

14.3 

1094 

1107 

1119 

1131 

1143 

1155 

1167 

1179 

1192 

1204 

14.4 

1087 

1099 

1111 

1123 

1136 

1148 

1160 

1172 

1184 

1196 

14  5 

1080 

1092 

1104 

1116 

1128 

1140 

1152 

1164 

1176 

1188 

14  6 

1073 

1085 

1097 

1109 

1120 

1132 

1144 

1156 

1168 

1180 

14.7 

1066 

1078 

1089 

1101 

1113 

1125 

1137 

1149 

1160 

1172 

14.8 

1058 

1070 

1082 

1094 

1105 

1117 

1129 

1141 

1152 

1164 

14.9 

1053 

1064 

1076 

1088 

1099 

1111 

1123 

1134 

1146 

1158 

15.0 

1046 

1057 

1069 

1081 

1092 

1104 

1116 

1127 

1139 

1150 

240 


METHODS  OF   ANALYSIS 


TABLE  17— Continued 


%C02 

T—  t 

500 

505 

510 

515 

520 

525 

530 

535 

540 

545 

550 

10.5 

1631 

1647 

1664 

1680 

1696 

1712 

1729 

1745 

1761 

1778 

1794 

10.6 

1616 

1632 

1648 

1664 

1681 

1697 

1713 

1729 

1745 

1761 

1778 

10.7 

1602 

1618 

1634 

1650 

1666 

1682 

1698 

1714 

1730 

1746 

1762 

10.8 

1588 

1603 

1619 

1635 

1651 

1667 

1683 

1699 

1714 

1730 

1746 

10.9 

1574 

1589 

1605 

1621 

1636 

1652 

1668 

1684 

1699 

1715 

1731 

11.0 

1560 

1576 

1591 

1607 

1622 

1638 

1654 

1669 

1685 

1700 

1716 

11.1 

1546 

1561 

1577 

1592 

1608 

1623 

1639 

1654 

1670 

1685 

1701 

11.2 

1533 

1548 

1564 

1579 

1594 

1610 

1625 

1640 

1656 

1671 

1686 

11.3 

1520 

1535 

1550 

1566 

1581 

1596 

1611 

1626 

1642 

1657 

1672 

11.4 

1510 

1525 

1540 

1555 

1570 

1585 

1600 

1615 

1630 

1645 

1660 

11.5 

1497 

1511 

1526 

1541 

1556 

1571 

1586 

1601 

1616 

1631 

1646 

11.6 

1484 

1499 

1514 

1529 

1543 

1558 

1573 

1588 

1608 

1618 

1632 

11.7 

1472 

1487 

1501 

1516 

1531 

1546 

1560 

1575 

1590 

1604 

1619 

11.8 

1461 

1475 

1490 

1504 

1519 

1534 

1548 

1563 

1577 

1592 

1607 

11.9 

1444 

1459 

1473 

1488 

1502 

1516 

1531 

1546 

1560 

1575 

1589 

12.0 

1438 

1452 

1466 

1481 

1495 

1509 

1524 

1538 

1552 

1567 

1581 

12.1 

1426 

1440 

1455 

1469 

1483 

1497 

1512 

1526 

1540 

1554 

1569 

12.2 

1415 

1429 

1443 

1457 

1472 

1485 

1499 

1514 

1528 

1542 

1556 

12.3 

1404 

1418 

1432 

1446 

1460 

1474 

1488 

1502 

1516 

1530 

1544 

12.4 

1393 

1406 

1420 

1434 

1440 

1462 

1476 

1490 

1504 

1518 

1532 

12.5 

1382 

1396 

1410 

1423 

1437 

1451 

1465 

1479 

1493 

1506 

1520 

12.6 

1372 

1386 

1399 

1413 

1427 

1441 

1454 

1468 

1482 

1495 

1509 

12.7 

1360 

1374 

1387 

1401 

1414 

1428 

1442 

1455 

1469 

1482 

1496 

12.8 

1350 

1364 

1377 

1389 

1404 

1417 

1431 

1445 

1459 

1472 

1485 

12.9 

1340 

1353 

1367 

1380 

1394 

1407 

1420 

1434 

1447 

1461 

1474 

13.0 

1330 

1343 

1357 

1370 

1383 

1397 

1410 

1423 

1436 

1450 

1463 

13.1 

1321 

1334 

1347 

1360 

1373 

1387 

1400 

1413 

1426 

1439 

1453 

13.2 

1312 

1325 

1338 

1351 

1364 

1377 

1390 

1403 

1416 

1429 

1443 

13.3 

1302 

1315 

1328 

1341 

1354 

1367 

1380 

1393 

1406 

1419 

1432 

13.4 

1293 

1305 

1318 

1331 

1344 

1357 

1370 

1383 

1396 

1409 

1422 

13.5 

1284 

1297 

1310 

1323 

1335 

1348 

1361 

1374 

1387 

1400 

1412 

13.6 

1275 

1287 

1300 

1313 

1326 

1338 

1351 

1364 

1377 

1389 

1402 

13.7 

1266 

1278 

1291 

1303 

1316 

1329 

1341 

1354 

1367 

1379 

1392 

13.8 

1257 

1269 

1282 

1294 

1307 

1319 

1332 

1344 

1357 

1370 

1382 

13.9 

1249 

1261 

1273 

1286 

1298 

1311 

1323 

1336 

1348 

1361 

1373 

14.0 

1240 

1252 

1265 

1277 

1290 

1302 

1314 

1327 

1339 

1352 

1364 

14.1 

1232 

1244 

1257 

1269 

1281 

1294 

1306 

1318 

1331 

1343 

1355 

14.2 

1224 

1236 

1248 

1261 

1273 

1285 

1297 

1310 

1322 

1334 

1346 

14.3 

1216 

1228 

1240 

1252 

1264 

1277 

1289 

1301 

1313 

1325 

1338 

14.4 

1208 

1220 

1232 

1244 

1256 

1268 

1280 

1293 

1305 

1317 

1329 

14.5 

1200 

1211 

1223 

1285 

1247 

1259 

1271 

1283 

1295 

1307 

1319 

14.6 

1192 

1204 

1216 

1228 

1240 

1252 

1264 

1275 

1287 

1299 

1311 

14.7 

1184 

1196 

1208 

1220 

1231 

1243 

1255 

1267 

1279 

1291 

1303 

14.8 

1176 

1188 

1200 

1211 

1223 

1235 

1247 

1258 

1270 

1282 

1294 

14.9 

1170 

1181 

1193 

1205 

1216 

1228 

1240 

1251 

1263 

1275 

1286 

15.0 

1162 

1176 

1185 

1197 

1200 

1220 

1232 

1243 

1255 

1267 

1278 

XXVI  I.       TABI.KS 


241 


TABLE  17— Continued 
Derivation 

The  flue  gas  is  assumed  to  contain  80.5%  nitrogen  and  no  carbon  monoxide, 
heat  is  taken  as  0.24. 

Let  a  -%  CO,  in  flue  gas 
b   =  %  oxygen  in  flue  gas 
c    =%  nitrogen  in  flue  gas  (80.5) 
W  =lbs.  of  dry  flue  gas  per  Ib.  of  carbon  burned 
L  =B.  T.  U.  lost  in  dry  flue  gas,  per  Ib.  of  carbon  burned 
L'  =B.  T.  U.  lost  in  dry  flue  gas,  per  Ib.  of  coal  burned 


The  specific 


Then  W 


lla+8b+7c 


3a 

L  =0.24  W  (T  -  t) 
L'=.57L 


MOISTURE  FACTOR' 


TABLE  18 

FOR  COMPUTING  LOSS  OF  HEAT  IN  FLUE  GAS  DUE  TO 
MOISTURE 


Based  on  Coal  Containing  6%  Hydrogen 

If  F  =  moisture  factor  as  found  in  this  table,  F'  =  temperature  factor  as  found  in  Table 
18-A,  A  =  B.  T.  U.  in  coal  as  fired,  and  Li  =  total  loss  of  heat  due  to  moisture, 

FxF/ 


%  MOISTURE 
IN  COAL 

.0 

.1 

.2 

.3 

.4 

.5 

.6 

.7 

.8 

.9 

10 

64.0 

64.1 

64.2 

64.3 

64.4 

64.5 

64.6 

64.7 

64.8 

64.9 

i     11 

65.0 

65.1 

65.2 

65.3 

65.4 

65.5 

65.6 

65.7 

65.8 

65.9 

12 

66.0 

66.1 

66.2 

66.3 

66.4 

66.5 

66.6 

66.6 

66.8 

66.9 

13 

67.0 

67.1 

67.2 

67.3 

67.4 

67.5 

67.6 

67.7 

67.8 

67.9 

14 

68.0 

68. 

68.2 

68.2 

68.4 

68.5 

68.6 

68.7 

68.8 

68.9 

15 

69.0 

69. 

69.2 

69.3 

69.4 

69.5 

69.6 

69.7 

69.8 

69.9 

16 

70.0 

70. 

70.2 

70.3 

70.4 

70.5 

70.6 

70.7 

70.8 

70.9 

17 

71.0 

71. 

71.2 

71.3 

71.4 

71.5 

71.6 

71.7 

71.8 

71.9 

18 

72.0 

72. 

72.2 

72.3 

72.4 

72.5 

72.6 

72.7 

72.8 

72.9 

19 

73.0 

73. 

73.2 

73.3 

73.4 

73.5 

73.6 

73.7 

73.8 

73.9 

20 

74.0 

74. 

74.2 

74.3 

74.4 

74.5 

74.6 

74.7 

74.8 

74.9 

21 

75.0 

75.1 

75.2 

75.3 

75.4 

75.5 

75.6 

75.7 

75.8 

75.9 

22 

76.0 

76.1 

76.2 

76.3 

76.4 

76.5 

76.6 

76.7 

76.8 

76.9 

23 

77.0 

77.1 

77.2 

77.3 

77.4 

77.5 

77.6 

77.7 

77.8 

77.9 

24 

78.0 

78.1 

78.2 

78.3 

78.4 

78.5 

78.6 

78.7 

78.8 

78.9 

25 

79.0 

79.1 

79.2 

79.3 

79.4 

79.5 

79.6 

79.7 

79.8 

79.9 

Derivation 

Let  M  -moisture  in  coal 
H  =  hydrogen  in  coal 
F  =  moisture  factor 
ThenF  -M+9  H-M+54 


242 


METHODS  OF  ANALYSIS 


TABLE  18-A 

'TEMPERATURE  FACTOR"  FOR  COMPUTING  LOSS  OF  HEAT  IN  FLUE  GAS  DUE 

TO  MOISTURE, 

Based  on  boiling  point  of  water  of  202°  F.  (at  5000  feet  elevation) 
The  use  of  this  factor  is  described  in  the  explanation  under  Table  18. 


TEMP. 

TEMPERATURE  (°F.)  OF  BOILER  ROOM 

TEMP. 

(°F.)  OF 

(°F.)  OF 

FT  TTF  OA<3 

FT  TTF  nAQ 

JL  AJ  \J  J-j  \jr/VO 

30 

40 

50 

60 

70 

80 

90 

100 

J~  J-J\J  1-J  \_T/\O 

330 

1209 

1199 

1189 

1179 

1169 

1159 

1149 

1139 

330 

340 

1213 

1203 

1193 

1183 

1173 

1163 

1153 

1143 

340 

350 

1218 

1208 

1198 

1188 

1178 

1168 

1158 

1148 

350 

360 

1223 

1213 

1203 

1193 

1183 

1173 

1163 

1153 

360 

370 

1228 

1218 

1208 

1198 

1188 

1178 

1168 

1158 

370 

380 

1232 

1222 

1212 

1202 

1192 

1182 

1172 

1162 

380 

390 

1237 

1227 

1217 

1207 

1197 

1187 

1177 

1167 

390 

400 

1242 

1232 

1222 

1212 

1202 

1192 

1182 

1172 

400 

410 

1246 

1236 

1226 

1216 

1206 

1196 

1186 

1176 

410 

420 

1251 

1241 

1231 

1221 

1211 

1201 

1191 

1181 

420 

430 

1256 

1246 

1236 

1226 

1216 

1206 

1196 

1186 

430 

440 

1260 

1250 

1240 

1230 

1220 

1210 

1200 

1190 

440 

450 

1265 

1255 

1245 

1235 

1225 

1215 

1205 

1195 

450 

460 

1270 

1260 

1250 

1240 

1230 

1220 

1210 

1200 

460 

470 

1275 

1265 

1255 

1245 

1235 

1225 

1215 

1206 

470 

480 

1279 

1269 

1259 

1249 

1239 

1229 

1219 

1209 

480 

490 

1284 

1274 

1264 

1254 

1244 

1234 

1224 

1214 

490 

500 

1289 

1279 

1269 

1259 

1249 

1239 

1229 

1219 

500 

510 

1293 

1283 

1273 

1263 

1253 

1243 

1233 

1223 

510 

520 

1298 

1288 

1278 

1268 

1258 

1248 

1238 

1228 

520 

530 

1303 

1293 

1283 

1273 

1263 

1253 

1243 

1233 

530 

540 

1307 

1297 

1287 

1277 

1267 

1257 

1247 

1237 

540 

550 

1312 

1302 

1292 

1282 

1272 

1262 

1252 

1242 

550 

560 

1317 

1307 

1297 

1287 

1277 

1267 

1257 

1247 

560 

570 

1322 

1312 

1302 

1292 

1282 

1272 

1262 

1252 

570 

580 

1326 

1316 

1306 

1296 

1286 

1276 

1266 

1256 

580 

590 

1331 

1321 

1311 

1301 

1291 

1281 

1271 

1261 

590 

600 

1336 

1326 

1316 

1306 

1296 

1286 

1276 

1266 

600 

610 

1340 

1330 

1320 

1310 

1300 

1290 

1280 

1270 

610 

620 

1345 

1335 

1325 

1315 

1305 

1295 

1285 

1275 

620 

630 

1350 

1340 

1330 

1320 

1310 

1300 

1290 

1280 

630 

640 

1354 

1344 

1334 

1324 

1314 

1304 

1294 

1284 

640 

650 

1359 

1349 

1339 

1329 

1319 

1309 

1299 

1289 

650 

30 

40 

50 

60 

70 

80 

90 

100 

Derivation 

If  T  =temp.  (°F.)  of  flue  gas,  t  =temp.  (°F.)  of  boiler  room,  w  =boiling  point  of  water  (202°  F 
at  5000  feet  elevation),  and  F'=factor  in  table, 

Then  F'  =  (w-t)+976.6  +  .47  (T-w) 


XXVII.       TABLES 


243 


TABLE  19 

CaO  IN  MILK  OF  LIME  OF  VARIOUS  DENSITIES  (15°C.) 
Blattner's  Table 

Milk  of  lime  made  up  with  sweet  water  will  show  only  about  85  per  cent,  of  the  CaO  given 
by  this  table. 


Degrees 
Brix 

Specific 
Gravity 

Grams  CaO 
per  Liter 

%CaO 
by  Weight 

Degrees 
Brix 

Specific 
Gravity 

Grams  CaO 
per  Liter 

%CaO 
by  Weight 

25 

1.107 

135 

12.2 

36 

.160 

203 

17.5 

26 

1.111 

141 

12.6 

37 

.165 

209 

17.9 

27 

1.116 

147 

13.2 

38 

.170 

215 

18.4 

28 

1.120 

153 

13.7 

39 

.175 

221 

18.8 

29 

1  125 

159 

14.1 

40 

.180 

228 

19.3 

30 

1.130 

165 

14.6 

41 

.185 

235 

19.8 

31 

1.135 

171 

15.1 

42 

.190 

242 

20.3 

32 

1.140 

177 

15.5 

43 

.195 

248 

20.8 

33 

1.145 

183 

16.0 

44 

.200 

255 

21.3 

34 

1.150 

189 

16.4 

45 

.205 

262 

21.7 

35 

1.155 

195 

16.9 

46 

.210 

269 

22.2 

244 


METHODS  OF   ANALYSIS 


TABLE  20 
EQUIVALENTS  OF  NORMAL  SOLUTIONS 


SUBSTANCE 

FORMULA 

MOLECULAR 
OR  ATOMIC 
WEIGHT 

NORMAL 
COEFFICIENTS 

g  per  Liter 

1  ml=g 

Ammonia 

NHa 

17.032 

17.032 

.01703 

Ammonium  sulphocyanate 

NH<CNS 

76.113 

76.113 

.07611 

Arsenious  cxide 

As2O3 

197.92 

*49.48 

*.  04948 

Barium  hydroxide 

Ba(OH)2.8H2O 

315.514 

157.757 

.  15776 

Benzoic  acid 

C6H,CO2H 

122.083 

122.083 

.  12208 

Calcium 

Ca 

40.07 

20.035 

.02003 

Calcium  carbonate 

CaCOs 

100.075 

50.037 

.05004 

Calcium  oxide 

CaO 

56.07 

28.035 

.02803 

Chlorine 

Cl 

35.46 

35.46 

.  03546 

Copper 
Hydrochloric  acid 

Cu 
HC1 

63.57 
36.468 

31.785 
36.468 

.03178 
.03647 

Iodine 

I 

126.92 

126.92 

.12692 

Nitric  acid 

HNOs 

63.016 

63.016 

.06202 

Potassium  permanganate 

KMnO< 

158.03 

*31.606 

*.  03151 

Potassium  sulphocyanate 

KCNS 

97.173 

97.173 

.09717 

Silver  nitrate 

AgNO, 

169.888 

169.888 

.16989 

Sodium  carbonate 

Na»COi 

106.005 

53.002 

.05300 

Sodium  chloride 

NaCl 

58.46 

58.46 

.05846 

Sodium  hydroxide 

NaOH 

40.008 

40.008 

.04001 

Sodium  oxalate 

Na2C2O4 

134.01 

*67.005 

*.  06700 

Sodium  thiosulphate 

Na?S2O3.5H>O 

248.20 

*248.20 

*.  24820 

Sulphuric  acid 

H..SO4 

98.076 

49.038 

.04904 

*As  oxidizing  or  reducing  agent. 


XXVII.       TABLES 


245 


TABLE  21 

PERCENTAGE  OF  AVAILABLE  GRANULATED  ON  DRY  SUBSTANCE  OF  SUGAR 
SOLUTIONS  (MOLASSES  PURITY  OF  60) 


Pur- 

.0 

.1 

.2 

.3 

.4 

.5 

.6 

.7 

.8 

.9 

Pur- 

ity 

ity 

60 

0.0 

.25 

'.5 

.75 

1.0 

1  25 

1.5 

1.75 

2.0 

2.25 

60 

61 

2.5 

2.75 

3.0 

3.25 

3.5 

3.75 

4.0 

4.25 

4.5 

4.75 

61 

62 

5.0 

5.25 

5.5 

o  .  75 

6.0 

6.25 

6.5 

6.75 

7.0 

7.25 

62 

63 

7.5 

7.75 

8.0 

8.25 

8.5 

8.75 

9.0 

9.25 

9.5 

9.75 

63 

64 

10.0 

10.25 

10.5 

10.75 

11.0 

11.25 

11.5 

11.75 

12.0 

12.25 

64 

65 

12.5 

12.75 

13.0 

13.25 

13.5 

13.75 

14.0 

14.25 

14.5 

14.75 

65 

66 

15.0 

15.25 

15.5 

15.75 

16.0 

16.25 

16.5 

16.75 

17.0 

17.25 

66 

67 

17.5 

17.75 

18.0 

18.25 

18.5 

18.75 

19.0 

19.25 

19.5 

19.75 

67 

68 

20.0 

20.25 

20.5 

20.75 

21.0 

21.25 

21.5 

21.75 

22.0 

22.25 

68 

69 

22.5 

22.75 

23.0 

23.25 

23.5 

23.75 

24.0 

24.25 

24.5 

24.75 

69 

70 

25.0 

25.25 

25.5 

25.75 

26.0 

26.25 

26.5 

26.75 

27.0 

27.25 

70 

71 

27.5 

27.75 

28.0 

28.25 

28.5 

28.75 

29.0 

29.25 

29.5 

29.75 

71 

72 

30.0 

30.25 

30.5 

30.75 

31.0 

31.25 

31.5 

31.75 

32.0 

32.25 

72 

73 

32.5 

32.75 

33.0 

33.25 

33.5 

33.75 

34.0 

34.25 

34.5 

34.75 

73 

74 

35.0 

35.25 

35.5 

35.75 

36.0 

36.25 

36.5 

36.75 

37.0 

37.25 

74 

75 

37.5 

37.75 

38.0 

38.25 

38.5 

38.75 

39.0 

39.25 

39.5 

39.75 

75 

76 

40.0 

40.25 

40.5 

40.75 

41.0 

41.25 

41.5 

41.75 

42.0 

42.25 

76 

77 

42.5 

42.75 

43.0 

43.25 

43.5 

43.75 

44.0 

44.25 

44.5 

44.75 

77 

78 

45.0 

45.25 

45.5 

45.75 

46.0 

46.25 

46.5 

46.75 

47.0 

47.25 

78 

79 

47.5 

47.75 

48.0 

48.25 

48.5 

48.75 

49.0 

49.25 

49.5 

49.75 

79 

80 

50.0 

50.25 

50.5 

50  75 

51.0 

51.25 

51.5 

51.75 

52.0 

52.25 

80 

81 

52.5 

52.75 

53.0 

53.25 

53  5 

53.75 

54.0 

54.25 

54.5 

54.75 

81 

82 

55.0 

55.25 

55.5 

55.75 

56.0 

56.25 

56.5 

56  75 

57.0 

57.25 

82 

83 

57.5 

57.75 

58.0 

58.25 

58.5 

58.75 

59.0 

59.25 

59.5 

59.75 

83 

84 

60.0 

60.25 

60.5 

60.75 

61.0 

61.25 

61.5 

61.75 

62.0 

62.25 

84 

85 

62.5 

62.75 

63.0 

63.25 

63.5 

63.75 

64.0 

64.25 

64.5 

64.75 

85 

86 

65.0 

65.25 

65.5 

65.75 

66.0 

66.25 

66.5 

66.75 

67.0 

67.25 

86 

87 

67.5 

67.75 

68.0 

68.25 

68.5 

68.75 

69.0 

69.25 

69.5 

69.75 

87 

88 

70.0 

70.25 

70.5 

70.75 

71.0 

71.25 

71.5 

71.75 

72.0 

72.25 

88 

89 

72.5 

72.75 

73.0 

73.25 

73.5 

73.75 

74.0 

74.25 

74.5 

74.75 

89 

90 

75.0 

75.25 

75.5 

75.75 

76.0 

76.25 

76.5 

76.75 

77.0 

77.25 

90 

91 

77.5 

77.75 

78.0 

78.25 

78.5 

78  75 

79.0 

79.25 

79.5 

79.75 

91 

92 

SO.O 

80.25 

80.5 

80.75 

81.0 

81.25 

81.5 

81.75 

82.0 

82.25 

92 

93 

82.5 

82.75 

83.0 

83.25 

83.5 

83.75 

84.0 

84.25 

84.5 

84.75 

93 

94 

85.0 

85.25 

85.5 

85.75 

86.0 

86.25 

86.5 

86.75 

87  0 

87.25 

94 

95 

87.5 

87.75 

88.0 

88.25 

88.5 

88.75 

89.0 

89.25 

89.5 

89:75 

95 

96 

90.0 

90.25 

90.5 

90.75 

91.0 

91.25 

91.5 

91.75 

92.0 

92.25 

96 

97 

92.5 

92.75 

93.0 

93.25 

93.5 

93.75 

94.0 

94.25 

94.5 

94.75 

97 

98 

95.0 

95.25 

95.5 

95.75 

96.0 

96.25 

96.5 

96.75 

97.0 

97.25 

98 

99 

97.5 

97.75 

98.0 

98.25 

98.5 

98.75 

99.0 

99.25 

99.5 

99.75 

99 

.0 

.1 

.2 

.3 

.4 

.5 

.6 

.7 

.8 

.9 

DERIVATION:— If  P -purity  and  F -granulated  factor,  F-2.5  (P-60). 


246 


METHODS  OF  ANALYSIS 


TABLE  22 

PERCENTAGE  OF  AVAILABLE  GRANULATED  ON  TOTAL  SUGAR  OF  SUGAR  SO- 
LUTIONS (MOLASSES  PURITY  OF  60) 

This  table  should  not  be  confused  with  Table  21,  which  is  the  one  mostly  employed  in  taking 
stock.  Table  22  is  intended  for  use  where  the  polarization  and  purity  of  a  product  are  known. 
E.  g.,  if  a  lot  of  10,000  Ibs.  of  raw  sugar  has  a  polarization  of  96 . 7  and  a  purity  of  97 . 1,  the  amount 
of  sugar  in  the  raw  sugar  is  10,000x96.7-^-100=9670  Ibs.  The  factor  corresponding  to  97.1  in 
Table  22  is  95 . 52.  The  "available  granulated"  is  then,  9670  x95 . 52  -100  =9237  Ibs. 


Pur- 

.0 

.1 

.2 

.3 

.4 

.5 

.6 

.7 

.8 

.9 

Pur- 

ity 

ity 

60 

0.00 

0.42 

0.83 

1.25 

1.66 

2.07 

2.48 

2.88 

3.29 

3.69 

60 

61 

4.10 

4.50 

4.90 

5.30 

5.70 

6.10 

6.49 

6.89 

7.28 

7.67 

61 

62 

8.06 

8.45 

8.84 

9.23 

9.62 

10.00 

10.38 

10.77 

11.15 

11.53 

62 

63 

11.90 

12.28 

12.66 

13.03 

13.41 

13.78 

14.15 

14.52 

14.89 

15.26 

63 

64 

15.62 

15.99 

16.36 

16.72 

17.08 

17.44 

17.80 

18.16 

18.52 

18.88 

64 

65 

19.23 

19.59 

19.94 

20.29 

20.64 

20.99 

21.34 

21.69 

22.04 

22.38 

65 

66 

22.73 

23.07 

23.41 

23.76 

24.10 

24.44 

24.77 

25.11 

25.45 

25.79 

66 

67 

26.12 

26.45 

26.79 

27.12 

27.45 

27.78 

28.11 

28.43 

28.76 

29.09 

67 

68 

29.41 

29.74 

30.06 

30.38 

30.70 

31.02 

31.34 

31.66 

31.98 

32.29 

68 

69 

32.61 

32.92 

33.24 

33.55 

33.86 

34.17 

34.48 

34.79 

35.10 

35.41 

69 

70 

35.71 

36.02 

36.32 

36.63 

36.93 

37.23 

37.54 

37.84 

38.14 

38.43 

70 

71 

38.73 

39.03 

39.33 

39.62 

39.92 

40.21 

40.50 

40.79 

41.09 

41.38 

71 

72 

41.67 

41.96 

42.24 

42.53 

42.82 

43.10 

43.39 

33.67 

43.96 

44.24 

72 

73 

44.52 

44.80 

45.08 

45.36 

45.64 

45.92 

46.20 

46.47 

46.75 

47.02 

73 

74 

47.30 

47.57 

47.84 

48.12 

48.39 

48.66 

48.93 

49.20 

49.47 

49.73 

74 

',5 

50.00 

50.27 

50.53 

50.80 

51.06 

51.32 

51.59 

51.85 

52.11 

52.37 

75 

76 

52.63 

52.89 

53.15 

53.41 

53.66 

53.92 

54.18 

54.43 

54.69 

54.94 

76 

77 

55.19 

55.45 

55.70 

55.95 

56.20 

56.45 

56.70 

56.95 

57.20 

57.45 

77 

78 

57.69 

57.94 

58.18 

58.43 

58.67 

58.92 

59.16 

59.40 

59.64 

59.89 

78 

79 

60.13 

60.37 

60.61 

60.85 

61.08 

61.32 

61.56 

61.79 

62.03 

62.27 

79 

80 

62.50 

62.73 

62.97 

63.20 

63.43 

63.66 

63.90 

64.13 

64.36 

64.59 

80 

81 

64.81 

65.04 

65.27 

65.50 

65.72 

65.95 

66.18 

66.40 

66.63 

66.85 

81 

82 

67.07 

67.30 

67.52 

67.74 

67.96 

68.18 

68.40 

68.62 

68.84 

69.06 

82 

83 

69.28 

69.49 

69.71 

69.93 

70.14 

70.36 

70.57 

70.79 

71.00 

71.22 

83 

84 

71.43 

71.64 

71.85 

72.06 

72.27 

72.49 

72.70 

72.90 

73.11 

73.32 

84 

85 

73.53 

73.74 

73.94 

74.15 

74.36 

74.56 

74.77 

74.97 

75.17 

75.38 

85 

86 

75.58 

75.78 

75.99 

76.19 

76.39 

76.59 

76.79 

76.99 

77.19 

77.39 

86 

87 

77.59 

77.78 

77.98 

78.18 

78.38 

78.57 

78.77 

78.96 

79.16 

79.35 

87 

88 

79.55 

79.74 

79.93 

80.12 

80.32 

80.51 

80.70 

80.89 

81.08 

81.27 

88 

89 

81.46 

81.65 

81.84 

82.03 

82.21 

82.40 

82.59 

82.78 

82.96 

83.15 

89 

90 

83.33 

83.52 

83.70 

83.89 

84.07 

84.25 

84.44 

84.62 

84.80 

84.98 

90 

91 

85.16 

85.35 

85.53 

85.71 

85.89 

86.07 

86.24 

86.42 

86.60 

86.78 

91 

92 

86.96 

87.13 

87.31 

87.49 

87.66 

87.84 

88.01 

88.19 

88.36 

88.54 

92 

93 

88.71 

88.88 

89.06 

89.23 

89.40 

89.57 

89.74 

89.91 

90.09 

90.26 

93 

94 

90.43 

90.60 

90.76 

90.93 

91.10 

91.27 

91.44 

91.61 

91.77 

91.94 

94 

95 

92.11 

92.27 

92.44 

92.60 

92.77 

92.93 

93.10 

93.26 

93.42 

93.59 

95 

96 

93.75 

93.91 

94.07 

94.24 

94.40 

94.56 

94.72 

94.88 

95.04 

95.20 

96 

97 

95.36 

95.52 

95.68 

95.84 

96.00 

96.15 

96.31 

96.47 

96.63 

96.78 

97 

98 

96.94 

97.09 

97.25 

97.41 

97.56 

97.72 

97.87 

98.02 

98.18 

98.33 

98 

99 

98.48 

98.64 

98.79 

98.94 

99.09 

99.25 

99.40 

99.55 

99.70 

99.85 

99 

.0 

.1 

.2 

.3 

.4 

.5 

.6 

.7 

.8 

.9 

DERIVATION:— If  P=  purity  and  F' =  granulated  factor,  F 


,    250  (P-60) 


XXVn.      TABLES 


247 


TABLE  23 
STANDARD  BEET  EXTRACTION 

Based  on  0.60%  total  losses  on  beets,  40%  elimination,  and  57  apparent  purity  of  molasses. 


%  SUGAR  IN  COSSETTES 

Cos- 

. 

Cos- 

sette 

sette 

Pur. 

Pur. 

13.0 

13.2 

13.4 

13.6 

13.8 

14.0 

14.2 

14.4 

14.6 

14.8 

79.0 

::>  -2-2 

75  27 

75.32 

75.38 

75.42 

75.48 

75.52 

75.57 

75.62 

75.67 

79.0 

79.1 

75.35 

75.41 

75.45 

75.52 

75.56 

75.61 

75.66 

75.71 

75.76 

75.80 

79.1 

79.2 

75.47 

75.52 

75.57 

75.63 

75.68 

75.73 

75.77 

75.82 

75.88 

75.92 

79.2 

79.3 

75.59 

75.64 

75.69 

75.76 

75.80 

75.85 

75.91 

75.95 

76.00 

76.04 

79.3 

79.4 

75.71 

75.76 

75.80 

75.87 

75.92 

75.97 

76.02 

76.06 

76.12 

76.16 

79.4 

79.5 

75.84 

75.89 

75.94 

76.00 

76.05 

76.10 

76.16 

76.19 

76.25 

76.29 

79.5 

79.6 

75.95 

76.00 

76.04 

76.11 

76.16 

76.21 

76.26 

76.30 

76.35 

76.40 

79.6 

79.7 

76.06 

76.11 

76.16 

76.22 

76.27 

76.32 

76.37 

76.41 

76.47 

76.51 

79.7 

79.8 

7.'.   Is 

76.24 

76.28 

7f,  :;o 

76.40 

76.45 

76.50 

76.54 

76.60 

76.64 

79.8 

7'.'  '.' 

76.32 

76.37 

76.42 

76.48 

76.53 

76.58 

76.64 

76.67 

76.73 

76.77 

79.9 

Sll     I) 

76.43 

76.48 

76.53 

76.60 

76.64 

76.70 

76.75 

76.79 

76.85 

76.88 

80.0 

80.1 

76.55 

76.60 

76.64 

76.71 

76.76 

76.81 

76.87 

76.90 

76.96 

77.00 

80.1 

80.2 

76.66 

76.71 

76.76 

76.83 

76.88 

76.93 

76.98 

77.02 

77.08 

77.12 

80.2 

80.3 

:•-,  7s 

76.84 

76.88 

76.95 

77.00 

77.05 

77.09 

77  13 

77.20 

77.24 

80.3 

80.4 

76.90 

76.95 

77.01 

77.07 

77.12 

77.17 

77.22 

77.25 

77.32 

77.36 

80.4 

80.5 

77.01 

77.07 

77.12 

77.18 

77.24 

77.28 

77.33 

77.38 

77.43 

77.48 

80.5 

80.6 

77.13 

77.18 

77.25 

77.29 

77.35 

77.39 

77.45 

77.50 

77.54 

77.59 

80.6 

80.7 

77.24 

77.30 

77.36 

77.41 

77.46 

77.51 

77.56 

77.61 

77.66 

77.71 

80.7 

80.8 

77.37 

77.42 

77.47 

77.52 

77.58 

77.63 

77.68. 

77.72 

77.77 

77.82 

80.8 

80.9 

77.48 

77.53 

77.59 

77.64 

77.69 

77.74 

77.79 

77.84 

77.89 

77.94 

80.9 

81.0 

77.60 

77.65 

77.70 

77.75 

77.81 

77.86 

77.91 

77.96 

78.t)0 

78.05 

81.0 

81.1 

77.71 

77.76 

77.82 

77.87 

77.92 

77.97 

78.02 

78.07 

78.12 

78.17 

81.1 

81.2 

77.82 

77.88 

77.93 

77.98 

78.04 

78.09 

78.14 

78.19 

78.23 

78.28 

81.2 

81.3 

77.95 

78.00 

78.06 

78.11 

78.16 

78.21 

78.26 

78.31 

78.36 

78.41 

81.3 

81.4 

78.05 

78.11 

78.16 

78.21 

78.27 

78.32 

78.37 

78.42 

78.46 

78.51 

81.4 

81.5 

78.17 

78.22 

78.28 

78.33 

78.38 

78.43 

78.48 

78.53 

78.58 

78.63 

81.5 

81.6 

78.28 

78.34 

78.39 

78.44 

78.50 

78.55 

78.60 

78.65 

78.69 

78.75 

81.6 

81.7 

78.40 

78.45 

78.51 

78.55 

78.61 

78.66 

78.71 

78.76 

78.81 

78.86 

81.7 

81.8 

78.51 

78.56 

78.62 

78.67 

78.73 

78.78 

78.83 

78.88 

78.93 

78.98 

81.8 

81  9 

78.63 

78.68 

78.74 

78.78 

78.84 

78.89 

78.94 

78.99 

79.04 

79.09 

81.9 

82.0 

78.74 

78.79 

78.85 

78.90 

78.96 

79.01 

79.06 

79.01 

79.16 

79.20 

82.0 

82  1 

78.85 

78.91 

78.96 

79.01 

79.07 

79.12 

79.17 

79.22 

79.27 

79.32 

82.1 

VJ     _' 

78.97 

79.02 

79.08 

79.13 

79.19 

79.24 

79.28 

79.34 

79.39 

79.44 

82.2 

82.3 

79.08 

79.14 

79.19 

79.24 

79.30 

79.35 

79.40 

79.45 

79.50 

79.55 

82.3 

82.4 

79.20 

• 

79.25 

79.31 

79.36 

79.42 

79.47 

79.52 

79.57 

79.62 

79.67 

82.4 

82.5 

79.30 

79.36 

79.41 

79.46 

79.52 

79.57 

79.62 

79.67 

79.72 

79.77 

82.5 

82.6 

79.42 

79.47 

79.53 

79.59 

79.64 

79.69 

79.74 

79.79 

79.84 

79.89 

82.6 

82.7 

79.52 

79.58 

79.64 

79.68 

79.77 

79.82 

79.87 

79.92 

79.97 

80.02 

82.7 

82.8 

79.65 

79.70 

79.76 

79.81 

79.87 

79.92 

79.97 

80.02 

80.07 

80.12 

82.8 

82.9 

79.75 

79.81 

79.86 

79.91 

79.97 

80.02 

80.07 

80.12 

80.17 

80.22 

82.9 

13.0 

13.2 

13.4 

13.6 

13.8 

14.0 

14.2 

14.4 

14.6 

14.8 

248 


METHODS  OF  ANALYSIS 


TABLE  23— Continued 
STANDARD  BEET  EXTRACTION 


%  SUGAR  IN  COSSETTES 

Cos- 

Cos- 

setfe 

sette 

Pur 

Pur. 

15.0 

15.2 

15.4 

15.6 

15.8 

16.0 

16.2 

16.4 

16.6 

16.8 

79.0 

75.71 

75.75 

75.78 

75.82 

75.86 

75.90 

75.93 

75.97 

76.01 

76.04 

79.0 

79.1 

75.84 

75.88 

75.92 

75.96 

76.00 

76.04 

76.07 

76.11 

76.15 

76.18 

79.1 

79.2 

75.96 

75.99 

76.02 

76.07 

76.11 

76.15 

76.18 

76.22 

76.26 

76.30 

,79.2 

79.3 

76.08 

76.12 

76.16 

76.20 

76.24 

76.28 

76.31 

76.35 

76.39 

76.42 

79.3 

79.4 

76.20 

76.23 

76.27 

76.31 

76.35 

76.39 

76.43 

76.47 

76.50 

76.54 

79.4 

79.5 

76.33 

76.37 

76.41 

76.45 

76.49 

76.53 

76.56 

76.60 

76.63 

76.67 

79.5 

79.6 

76.44 

76.48 

76.51 

76.55 

76.59 

76.63 

76.67 

76.71 

76.74 

76.78 

79.6 

79.7 

76.55 

76.59 

76.63 

76.67 

76.70 

76.75 

76.78 

76.82 

76.86 

76.89 

79.7 

79.8 

76.68 

76.72 

76.76 

76.80 

76.83 

76.88 

76.91 

76.95 

76.98 

77.02 

79.8 

79.9 

76.81 

76.85 

76.88 

76.93 

76.97 

77.01 

77.04 

77.08 

77.12 

77.15 

79.9 

80.0 

76.92 

76.96 

77.00 

77.04 

77.09 

77.13 

77.16 

77.20 

77.24 

77.27 

80.0 

80.1 

77.04 

77.08 

77  .  12 

77.16 

77.20 

77.24 

77.27 

77.31 

77.35 

77.38 

80.1 

80.2 

77.16 

77.20 

77.24 

77.28 

77.32 

77.36 

77.40 

77.43 

77.47 

77.51 

80.2 

80.3 

77.28 

77.32 

77.36 

77.40 

77.44 

77.48 

77.51 

77.55 

77.58 

77.62 

80.3 

80.4 

77.40 

77.44 

77.48 

77.52 

77.57 

77.61 

77.64 

77.67 

77.71 

77.75 

80.4 

80.5 

77.52 

77.56 

77.60 

77.64 

77.68 

77.72 

77.75 

77.78 

77.82 

77.87 

80.5 

80.6 

77.63 

77.67 

77.71 

77.75 

77.79 

77.84 

77.87 

77.90 

77.95 

77.98 

80.6 

80.7 

77  .  75 

77.79 

77.83 

77.87 

77.91 

77.95 

77.98 

78.02 

78.07 

78.10 

80.7 

80.8 

77.85 

77.90 

77.94 

77.99 

78.03 

78.07 

78.11 

78.14 

78.18 

78.21 

80.8 

80.9 

77.98 

78.02 

78.06 

78.10 

78.14 

78.19 

78.23 

78.26 

78.30 

78.33 

80.9 

81.0 

78.09 

78.13 

78.18 

78.22 

78.26 

78.30 

78.34 

78.37 

78.41 

78.44 

81.0 

81.1 

78.21 

78.25 

78.29 

78.33 

78.37 

78.41 

78.46 

78.49 

78.53 

78.56 

81.1 

81.2 

78.32 

78.37 

78.41 

78.45 

78.49 

78.53 

78.57 

78.60 

78.64 

78.68 

81.2 

81.3 

78.45 

78.49 

78.53 

78.57 

78.61 

78.65 

78.69 

78.73 

78.76 

78.80 

81.3 

81.4 

78.55 

78.60 

78.64 

78.68 

78.72 

78.76 

78.80 

78.84 

78.87 

78.91 

81.4 

81.5 

78.64 

78.69 

78.73 

78.77 

78.81 

78.85 

78.89 

78.92 

78.97 

79.02 

81.5 

81.6 

78.79 

78.83 

78.87 

78.91 

78.95 

78.99 

79.03 

79.06 

79.10 

79.14 

81.6 

81.7 

78.90 

78.94 

78.98 

79.02 

79.06 

79.11 

79.15 

79.18 

79.22 

79.25 

81.7 

81.8 

79.02 

79.06 

79.10 

79.14 

79.18 

79.22 

79.27 

79.30 

79.34 

79.37 

81.8 

81.9 

79.13 

79.17 

79.21 

79.25 

79.29 

79.34 

79.38 

79.41 

79.44 

79.49 

81.9 

82.0 

79.25 

79.29 

79.33 

79.37 

79.41 

79.46 

79.49 

79.53 

79.56 

79.60 

82.0 

82.1 

79.36 

79.40 

79.44 

79.49 

79.54 

79.59 

79.63 

79.64 

79.69 

79.72 

82.1 

82.2 

79.48 

79.52 

79.56 

79.60 

79.64 

79.69 

79.73 

79.76 

79.79 

79.83 

82.2 

82.3 

79.59 

79.63 

79.67 

79.72 

79.77 

79.81 

79.85 

79.88 

79.91 

79  .  95 

82.3 

82.4 

79.71 

79.75 

79.79 

79.83 

79.87 

79.91 

79.95 

79.99 

80.02 

80.06 

82.4 

82.5 

79.81 

79.85 

79.89 

79.94 

79.99 

80.03 

80.07 

80.10 

80.14 

80.17 

82.5 

82.6 

79.93 

79.97 

80.01 

80.05 

80.10 

80.14 

80.18 

80.21 

80.25* 

80.29 

82.6 

82.7 

80.03 

80.07 

80.12 

80.16 

80.20 

80.24 

80.29 

80.32 

80.36 

80.39 

82.7 

82.8 

80.16 

80.20 

80.24 

80.28 

80.32 

80.37 

80.41 

80.44 

80.48 

80.52 

82.8 

82.9 

80.26 

80.31 

80.35 

80.39 

80.43 

80.47 

80.52 

80.55 

80.59 

80.62 

82.9 

15.0 

15.2 

15.4 

15.6 

15.8 

16.0 

16.2 

16.4 

16.6 

16.8 

XXVII.       TABLES 


249 


TABLE  23 — Continued 
STANDARD  BEET  EXTRACTION 


%  SUGAR  IN  COSSETTES 

Cos- 

Cos- 

sett  e 

sette 

Pur. 

Pur. 

13.0 

13.2 

13.4 

13.6 

13.8 

14.0 

14.2 

14.4 

14.6 

14.8 

83.0 

79.85 

79.90 

79.96 

80.01 

80.06 

80.12 

80.17 

80.22 

80.27 

80.32 

83.0 

83.1 

79.94 

79.99 

80.06 

80.10 

80.15 

80.20 

80.26 

80.31 

80.36 

80.41 

83.1 

83  .  2 

80.08 

80.13 

80.19 

80.24 

80.29 

80.35 

80.40 

80.45 

80.50 

80.55 

83.2 

83.3 

80.18 

80.23 

80.29 

80.34 

80.39 

80.45 

80.50 

80.55 

80.60 

80  65 

83.3 

83  4 

80.30 

80.35 

80.41 

80.45 

80.49 

80.57 

80.62 

80.67 

80.72 

80.77 

83.4 

83.5 

80.41 

80.46 

80.52 

80.57 

80.62 

80.68 

80.73 

80.78 

80.83 

80.88 

83.5 

83.6 

80.51 

80.57 

80.63 

80.68 

80.73 

80.79 

80.84 

80.89 

80.91 

80.99 

83.6 

83.7 

80.63 

80.68 

80.74 

80.79 

80.84 

80.90 

80.95 

81.00 

81.05 

81.10 

83.7 

83.8 

80.74 

80.80 

80.86 

80.91 

80.95 

81.02 

81.07 

81.12 

81.17 

81.22 

83.8 

83.9 

80.84 

80.88 

80.95 

80.99 

81.04 

81.10 

81.15 

81.20 

81.26 

81.31 

83.9 

84.0 

80.93 

80.99 

81.05 

81.10 

81.15 

81.21 

81.26 

81.31 

81.36 

81.41 

84.0 

84.1 

81.05 

81.10 

81.16 

81.21 

81.26 

81.32 

81.37 

81.42 

81.47 

81.53 

84.1 

84.2 

81.16 

81.22 

81.28 

81.33 

81.38 

81.42 

81.49 

81.54 

81.59 

81.64 

84.2 

84.3 

81.27 

81.32 

81.35 

81.43 

81.47 

81.52 

81.57 

81.65 

81.70 

81.75 

84.3 

M    1 

81.36. 

81.42 

81.48 

81.53 

81.59 

81.64 

81.69 

81.74 

81.79 

81.85 

84.4 

84.5 

81.48 

81.53 

81.59 

81.64 

81.70 

81.75 

81.80 

81.85 

81.90 

81.95 

84.5 

M  r, 

81.58 

81.64 

81.70 

81.75 

81.81 

81.86 

81.91 

81.96 

82.01 

82.06 

84.6 

84.7 

81.70 

81.75 

81.81 

81.86 

81.92 

81.97 

82.03 

82.08 

82.13 

82.18 

84.7 

M    v 

81.80 

81.85 

81.92 

81.97 

82.03 

82.08 

82.13 

"82.18 

82.23 

82.28 

84.8 

84.9 

81.91 

81.96 

82.02 

82.07 

82.13 

82.18 

82.24 

82.29 

82.34 

82:39 

84.9 

85.0 

82.00 

82.06 

82.12 

82.17 

82.23 

82.28 

82.33 

82.38 

82.43 

82.48 

85.0 

85.1 

82.11 

82.16 

82.22 

82.27 

82.33 

82.39 

82.44 

82.49 

82.54 

82.59 

85.1 

85.2 

82.22 

82.28 

82.34 

82.39 

82.45 

82.50 

82.55 

82.60 

82.66 

82.71 

85.2 

85.3 

82.33 

82.38 

82.44 

82.49 

82.55 

82.60 

82.65 

82.70 

82.75 

82.80 

85.3 

85.4 

82.43 

82.49 

82.55 

82.60 

82.65 

82.71 

82.76 

82.81 

82.86 

82.91 

85.4 

v,  :, 

82.53 

82.58 

82.64 

82.69 

82.75 

82.80 

82.85 

82.91 

82.96 

83.01 

85.5 

85.6 

82.63 

82.69 

82.75 

82.80 

82.86 

82.91 

82.96 

83.02 

83.07 

83.12 

85.6 

85.7 

82.74 

82.79 

82.88 

82.90 

82.96 

83.02 

83.07 

83.12 

83.17 

82.23 

35.7 

85.8 

82.84 

82.89 

82.96 

83.01 

83.07 

83.12 

83.17 

83.23 

83.28 

83.33 

85.8 

85.9 

82.94 

82.99 

83.05 

83.10 

83.17 

83.20 

83.27 

83.32 

83.37 

83.43 

85.9 

86.0 

83  03 

83  09 

83.15 

83.20 

83.21 

83.32 

83.37 

83.42 

83.47 

83.52 

86.0 

86.1 

83.16 

83.21 

83.27 

83.32 

83.39 

83.44 

83.49 

83.54 

83.59 

83.65 

86.1 

86.2 

83.26 

83.32 

83.38 

83.43 

83.49 

83.54 

83.59 

83.65 

83.70 

83.75 

86.2 

86.3 

83.35 

83.40 

83.46 

83.52 

83.58 

83.63 

83.68 

83.73 

83.78 

83.84 

86.3 

86.4 

83.45 

83.51 

83.57 

83.62 

83.68 

83  .  73 

83.78 

83.83 

83.89 

83.95 

86.4 

86.5 

83.57 

83.62 

83.68 

83.74 

83.80 

83.85 

83.90 

83.95 

84.01 

84.06 

86.5 

86.6 

83.65 

83.71 

83.77 

83.82 

83.88 

83.94 

83.99 

84.04 

84.09 

84.15 

86.6 

86.7 

83.76 

83.81 

83.87 

83.93 

83.99 

84.04 

84.09 

84.15 

84.20 

84.25 

86.7 

86.8 

83.86 

83.92 

83.98 

84.03 

84.09 

84.15 

84.19 

84.25 

84.30 

84.35 

86.8 

86.9 

83.96 

84.01 

84.07 

84.13 

84.19 

84.24 

84.29 

84.35 

84.40 

84.45 

86.9 

13.0 

13.2 

13.4 

13.6 

13.8 

14.0 

14.2 

14.4 

14.6 

14.8 

250 


METHODS  OF  ANALYSIS 


TABLE  23— Continued 
STANDARD  BEET  EXTRACTION 


%  SUGAR  IN  COSSETTES 

Cos- 

Cos- 

sette 

sette 

Pur. 

Pur. 

15.0 

15.2 

15.4 

15.6 

15.8 

16.0 

16.2 

16.4 

16.6 

16.8 

83.0 

80.36 

80.40 

80.44 

80.49 

80.54 

80.58 

80.63 

80.67 

80.69 

80.72 

83.0 

83.1 

80.46 

80.50 

80  .  54 

80.58 

80.63 

80.67 

80.71 

80.74 

80.79 

80.82 

83.1 

83.2 

80.59 

80.63 

80.67 

80.72 

80.76 

80  80 

80.84 

80.88 

80.92 

80.95 

83.2 

83.3 

80.70 

80.74 

80.78 

80.82 

80.86 

80.91 

80.95 

80.98 

81.03 

81.07 

83.3 

83.4 

80.80 

80.85 

80.89 

80.94 

80.99 

81.03 

81.07 

81.10 

81.14 

81.18 

83.4 

83.5 

80.93 

80.97 

81.01 

81.05 

81.09 

81  .  14 

81.18 

81.21 

81.26 

81.30 

83.5 

83.6 

81.03 

81.07 

81.12 

81.16 

81.20 

81.24 

81.28 

81.31 

81.36 

81.40 

83.6 

83.7 

81.15 

81.19 

81.23 

81.27 

81.32 

81  .  37 

81.41 

81.44 

81.48 

81.52 

83.7 

83.8 

81.26 

81.30 

81.35 

81.39 

81.44 

81.48 

81.52 

81.55 

81.59 

81.63 

83.8 

83.9 

81.35 

81.39 

81.43 

81.48 

81.53 

81.57 

81.61 

81.64 

81.68 

81.71 

83.9 

84.0 

81.46 

81.50 

81.54 

81.58 

81.62 

81.67 

81.71 

81.74 

81.79 

81.82 

84.0 

84.1 

81.57 

81.61 

81.65 

81.70 

81.75 

81.78 

81.81 

81.85 

81.89 

81.93 

84.1 

84.2 

81.68 

81.73 

81.77 

81.81 

81.85 

81.90 

81.94 

81.98 

82.02 

82.06 

84.2 

84.3 

81.79 

81.83 

81.87 

81.91 

81.95 

82.00 

82.04 

82.08 

82.12 

82.16 

84.3 

84.4 

81.88 

81.93 

81.97 

82.02 

82.06 

82.10 

82.15 

82.18 

82.22 

82.25 

84.4 

84.5 

82.00 

82.04 

82.09 

82.14 

82.18 

82.22 

82.26 

82.30 

82.34 

82.37 

84.5 

84.6 

82.11 

82.16 

82.21 

82.26 

82.29 

82.32 

82.36 

82.40 

82.44 

82.48 

84.6 

84.7 

82.23 

82.27 

82.31 

82.36 

82.39 

82.44 

82.49 

82.53 

82.57 

82.59 

84.7 

84.8 

82.33 

82.38 

82.42 

82.47 

82.51 

82.55 

82.59 

82.63 

82.65 

82.70 

84.8 

84.9 

82.43 

82.48 

82.52 

82.56 

82.60 

82.65 

82.69 

82.73 

82.77 

82.81 

84.9 

85.0 

82.53 

82.57 

82.62 

82.66 

82.70' 

82.75 

82.79 

82.83 

82.87 

82.91 

85.0 

85.1 

82.63 

82.68 

82.72 

82.77 

82.81 

82.86 

82.91 

82.95 

82.98 

83.03 

85.1 

85.2 

82.75 

82.79 

82.84 

82.89 

82.93 

82.97 

83.01 

83.04 

83.08 

83.12 

85.2 

85.3 

82.86 

82.91 

82.95 

82.99 

83.03 

83.08 

83.11 

83.15 

83.19 

83.25 

85.3 

85.4 

82.96 

83.00 

83.05 

83.09 

83.13 

83.18 

83.23 

83.26 

83.30 

83.34 

85.4 

85.5 

83.06 

83.11 

83.15 

83.19 

83.23 

83.28 

83.32 

83.35 

83.39 

83.43 

85.5 

85.6 

83.17 

83.21 

83.25 

83.30 

83.34 

83.38 

83.42 

83.45 

83.49 

83.54 

85.6 

85.7 

83.28 

83.33 

83.38 

83.41 

83.46 

83.50 

83.53 

83.57 

83.61 

83.65 

85.7 

85.8 

83.37 

83.42 

83.46 

83.50 

83.55 

83.59 

83.64 

83.67 

83.71 

83.75 

85.8 

85.9 

83.48 

83.53 

83.57 

83.61 

83.65 

83.69 

83.74 

83.77 

83.81 

83.85 

85.9 

86.0 

83.57 

83.61 

83.65 

83.70 

83.74 

83.78 

83.83 

83.86 

83.90 

83.94 

86.0 

86.1 

83.70 

83.75 

83.79 

83.83 

83.88 

83.92 

83.97 

84.00 

84.04 

84.08 

86.1 

86.2 

83.80 

83.84 

83.88 

83.93 

83.97 

84.02 

84.06 

84.10 

84.14 

84.17 

86.2 

86.3 

83.89 

83.94 

83.98 

84.02 

84.07 

84.11 

84.15 

84.18 

84.23 

84.27 

86.3 

86.4 

83.99 

84.03 

84.08 

84.13 

84.17 

84.21 

84.25 

84.28 

84.32 

84.36 

86.4 

86.5 

84.10 

84.15 

84.19 

84.24 

84.28 

84.33 

84.37 

84.40 

84.44 

84.48 

86.5 

86.6 

84.20 

84.25 

84.30 

84.34 

84.39 

84.43 

84.46 

84.49 

84.53 

84.58 

86.6 

86.7 

84.30 

84.35 

84.39 

84.43 

84.47 

84.51 

84.55 

84.59 

84.64 

84.68 

86.7 

86.8 

84.40 

84.45 

84.49 

84.53 

84.58 

84.62 

84.66 

84.70 

84.74 

84.78 

86.8 

86.9 

84.50 

84.54 

84.59 

84.63 

84.68 

84.72 

84.76 

84.80 

84.84 

84.88 

86.9 

15.0 

15.2 

15.4 

15.6 

15.8 

16.0 

16.2 

16.4 

16.6 

16.8 

Derivation 

Let  S  =  %  sugar  in  cossettes,  P=  apparent  purity  of  cossettes,  and  X=standard  extraction. 
Also  let  J=apparent  purity  of  purified  juice,  and  G=granulated  factor,  %  on  sugar. 


Then  J 


100  P 
4P+60 


10,000  (J -57) 
43  J 


X  = 


G  (S-.60) 


XXVII.      TABLES 


251 


TABLE  24 
STANDARD  STEFFEN  EXTRACTION 

Based  on  58  tree  purity  of  "molasses  produced  from  Steffen,"  and  a  total  loss  of  5.25%  of 
the  original  sugar  in  the  molasses  worked. 


True 

True 

Pur. 
of 

.0 

.1 

.2 

.3 

.4 

.5 

.6 

.7 

.8 

.9 

PIT. 
of 

Pert. 

Pfr'. 

Washeo 

Washed 

Cake 

Cake 

80 

81 

62.04 

64.06 

62.24 
64.26 

62.45 
64.46 

62.65 
64.66 

62.85 
64.85 

63.05 
65.05 

63.26 
65.25 

63.46 
65.44 

63.66 
65.64 

63.86 
65.83 

80 
81 

82 

66.03 

66.22 

66.42 

66.61 

66.80 

67.00 

67.19 

67.38 

67.57 

67.76 

82 

83 

67.95 

68.13 

68.33 

68.53 

68.71 

68.89 

69.08 

69.27 

69.46 

69.64 

83 

84 

69.84 

70.01 

70.20 

70.38 

70.57 

70.75 

70.93 

71.11 

71.30 

71.48 

84 

85 

71.67 

71.84 

72.02 

72.20 

72.38 

72.56 

72.74 

72.91 

73.10 

73.26 

85 

86 

73.45 

73.62 

73.80 

73.98 

74.15 

74.33 

74.50 

74.67 

74.85 

75.02 

86 

87 

75.20 

75.37 

75.54 

75.71 

75.89 

76.06 

76.23 

76.40 

76.57 

76.73 

87 

88 

76.91 

77.08 

77.24 

77.41 

77.58 

77.75 

77.91 

78.08 

78.25 

78.41 

88 

89 

78.58 

78,75 

78.91 

79.07 

79.24 

79.40 

79.56 

79.72 

79.89 

80.04 

89 

90 

80.21 

80.38 

80.53 

80.70 

80.85 

81.01 

81.17 

81.34 

81.49 

81.64 

90 

91 

81.81 

81.97 

82.12 

82.29 

82.44 

82.59 

82.75 

82.91 

83.06 

83.22 

91 

92 

83.38 

83.52 

83.68 

83.83 

83.99 

84.14 

84.29 

84.45 

84.60 

84.75 

92 

93 

84.90 

85.05 

85.20 

85.36 

85.50 

85.65 

85.80 

85.95 

86.10 

86.25 

93 

94 

86.40 

86.54 

86.69 

86.84 

86.99 

87.13 

87.28 

87.42 

87.57 

87.72 

94 

95 

87.86 

88.01 

88.15 

88.30 

88.44 

88.58 

88.73 

88.87 

89.01 

89.16 

95 

.0 

.1 

.2 

3 

.4 

.5 

.6 

.7 

.8 

.9 

Derivation 

Let  W  =true  purity  of  perfectly  washed  cake 
Y  =standard  Steffen  extraction 

9475  (W-58)    225.6  (W-58) 


Then  Y 


42  W 


W 


TABLE  25 
SPECIFIC  GRAVITY  OF  VARIOUS  MATERIALS 

WEIGHT 
IN  POUNDS 
OF  ONE 
CUBIC  FT. 

40-42 

37-40 

40-50 

50-52 


Beets 

Beet  pulp,  fresh 

Beet  pulp,  fermented. . 
Coal  (Colorado  lignite) 

Coke 

Lime,  burned 

Limestone 

Molasses 

Sugar,  raw 

Sugar,  white 


27 
50-60 

90 

90 
50-55 

55 


TRUE 
SP.  GR. 

•Sugar 1 .591 

Lime,  burned 2 . 30-4 . 20 

Limestone,  usually .  .  2 . 65-2 . 70 


252 


METHODS  OF  ANALYSIS 


TABLE  26 
INTERNATIONAL  ATOMIC  WEIGHTS,  1920 


Symbol 

Atomic 
Weight 

Symbol 

Atomic 
Weight 

Aluminum 

Al 

27  1 

M^olybdenum                

Mo 

96  0 

Antimony 

Sb 

ion  2 

Neodymium               

Nd 

144  3 

Argon     

A 

39  9 

Neon            

Ne 

20.2 

Ars6nic 

A« 

74  96 

Nickel                       

Ni 

58  68 

Barium 

Fla 

137  37 

Niton  (radium  emanation)  .  . 

Nt 

222  4 

Bismuth 

Bi 

208  0 

Nitrogen                

N 

14  008 

Boron 

B 

10  9 

Osmium                

Os 

190  9 

Bromine        

Br 

79  92 

Oxvffen                      

o 

16  00 

Cadmium          •            • 

Cd 

112  40 

Palladium    .       

Pd 

106  7 

Caesium            

Cs 

132  81 

Phosphorus         

p 

31  04 

Calcium             

On 

40  07 

Platinum               

Pt 

195  2 

Carbon            

c 

12  005 

Potassium           

K 

39  10 

Cerium          

CP 

140  25 

Praseodymium   

Pr 

140  9 

Chlorine          

Cl 

35  46 

Radium             

Ra 

226  0 

Chromium      

Cr 

52  0 

Rhodium             

Rh 

102  9 

Cobalt               

Co 

58  97 

Rubidium                  

Rb 

85  45 

Columbium     

Cb 

93  1 

Ruthenium                

Ru 

101  7 

Copper              

Cu 

63  57 

Samarium               

Sa 

150  4 

Dysprosium  
Erbium            

£ry 

162.5 
167  7 

Scandium  
Selenium               

Sc 

Se 

44.1 
79  2 

Europium  
Fluorine        

Eu 
F 

152.0 
19  0 

Silicon  
Silver                     

Si 
Ag 

28.3 
107.88 

Gadolinium     

Gd 

157  3 

Sodium                

Na 

23.00 

Gallium       

Ga 

70  1 

Strontium               

Sr 

87.63 

Germanium  

Ge 

72  5 

Sulfur                  

s 

32.06 

Glucinum  

Gl 

9  1 

Tantalum            

Ta 

181.5 

Gold         

Au 

197  2 

Tellurium                

Te 

127.5 

Helium     

He 

4  00 

Terbium                

Tb 

159.2 

Holmium  

Ho 

163  5 

Thallium           

Tl 

204.0 

Hydrogen  

H 

1  008 

Thorium          

Th 

232.15 

Indium  

In 

114  8 

Thulium      

Tm 

168.5 

Iodine    

I 

126  92 

Tin         

Sn 

118.7 

Iridium  

Ir 

193  1 

Titanium  

Ti 

48.1 

Iron 

FP 

55  84 

Tungsten                          .... 

W 

184.0 

Krypton  

Kr 

82  92 

Uranium  

U 

238.2 

Lanthanum     .  .    . 

La 

139  0 

Vanadium                            .  . 

V 

51.0 

Lead  

Pb 

207  20 

Xenon     

Xe 

130.2 

Lithium  

Li 

6  94 

Ytterbium  (Neoytterbium)  . 

Yb 

173.5 

Lutecium    

Lu 

175  0 

Yttrium                    

Yt 

89.33 

Magnesium       .  .  . 

Me 

24  32 

Zinc                                 

Zn 

65.37 

Manganese        .   . 

Mn 

54  93 

Zirconium                      

Zr 

90.6 

Mercury  

Hg 

200  6 

INDEX 


Acetic  acid,  dilute 

for  lime  cake   188 

for  saccharate  cake   1S8 

Acid   insoluble    92 

Acid,    standard    193 

Air  compressor    178 

Air    entering    furnaces,    temper- 
ature       75 

Alkali,    standard    193 

Alkalinity     11 

Alpha-naphthol    188 

detection  of  sugar  by 14,  37 

Alumina  cream    188 

Aluminum...  108,  109,  118,  134,  136 

discs     105,  168 

dishes    169 

Ammonia,  determination    123 

total  nitrogen  as  95 

Ammonium  carbonate   189 

molybdate    112 

nitrate 112 

oxalate    189 

Apparatus    168 

standardization  of 179 

Apparent  purity   6,  106 

table  of  factors  214 

Arsenic,  in   sulphur   150 

Asbestos,  preparation  of 94 

Ash   9,  128,  149,  156 

lixiviated    10,  93,  107 

sulphated    9 

Ash    analysis    107 

aluminum    108,  109 

calcium     109 

carbonic  acid    113 

chlorine    Ill 

hypothetical  combinations   . . .  113 

iron    '..108,  109 

lixiviated  ash    107 

magnesium    109 

phosphoric    acid    112 

potassium     110 

silica  and  insoluble   107 

sodium    110 

statement  of  analysis    114 

sulphuric   acid    112 


Ashes 

analysis    131 

preparation  of  samples  74 

sampling    73 

Atomic  weights,  table   252 

Bacteriological     examination    of 

water     139 

Balances     168 

Barium     chloride,     general     re- 
agent     189 

for    standardizing    soap    solu- 
tion     ."189 

Barium  oxide   199 

Basic  acetate  separation    108 

Battery  supply  water   141 

Baume,  of  molasses  101 

hydrometers    184 

scale    185 

table    201 

test    101 

Beets   (see  also  "cossettes") 

detn.  of  purity    17,  106 

detn.  of  sugar 17,  105,  106 

preparation  of  sample  102 

rasping  of   103 

Beet  laboratory  tests    102 

Beet  rasp,  see  "rasp." 

Beet  tailings   18 

Benzoic  acid   193 

Blow-up   thick  juice,   see  "thick 
juice." 

Boiler  house  control   72 

bibliography    79 

Boiler   water    38,     84 

Brix    1 

direct   method    1 

double  dilution  method 2 

table    201 

Burettes   181 

Calcium 109,  118,  134,  137,  143 

detn.  as  oxide 135 

detn.  as  sulphate 135 

volumetric  method   137 

Calcium  acetate  123 

Calcium  oxalate  scale  104 

Calorific  value    .  .  .130 


254 


IN  DEX 


Calorimeters    130,  186 

Campaign  average  samples.  140,  141 

CaO  by  soap  solution 13 

tables    224,  226 

CaO  by  titration   12 

CaO,   sugar-soluble   49 

Capsules    168 

covers    168 

Carbon    124 

fixed     129 

Carbon    dioxide,    see    "carbonic 
acid." 

Carbonator     169 

Carbonic  acid 

113,   121,  138,  145,  161 

Caustic  soda  199 

Chlorine,  detn.  97,  111,  119,  143 

Clerget    formula    6 

Coal    126 

bibliography    132 

preparation  of  samples. .  .73,  126 

sampling    72,  126 

Coal   analysis    128 

ash    .*. 128 

calorific   value    130 

•     fixed  carbon    129 

moisture     128 

sulphur   129 

volatile  matter  128 

Cochineal    190 

Coke    126 

bibliography    132 

preparation  of  samples 127 

sampling     127 

Coke  analysis,   see  "coal  analy- 
sis." 

Cold   water  digestion 103,  105 

Combinations,   hypothetical 

99,   113,  145 

Condensed    waters     37,     84 

Cooler     169,  177 

solution  for 47 

tests     57 

Copper,   determination    9,  116 

Cossettes 16 

Cotton  seed  cake   157 

analysis     158 

moisture 158 

prepn.  of  samples 157 

protein    1 5S 

sampling     157 


Crude  fat    ,...67,  155 

Crude  fiber    156 

Crude  potash   90 

analysis,     see    "crude    potash 
analysis." 

as  sacked   85,  86< 

preparation  of  samples 90,  92 

sampling  90 

Crude  potash  analysis 92 

acid  insoluble 92> 

chlorine    97 

complete  analysis  97 

general   92j 

hydrosulphuric  acid   98 

hypothetical  combinations  ...  99 

lixiviated  ash  93 

moisture     92 

nitrogen    95 

potash     93 

screen  test 97 

sulphuric  acid    98 

total  alkali  as  CQ2 97 

water  insoluble   93 

Crude  protein   151,  158 

Crusher    170,   177,  178 

Cupric  oxide  tables 223 

Cuprous  chloride 191 

Deposits,  see  "scales." 

Desiccators   2,  33 

Diatomaceous  earth   147 

apparent  specific  gravity 147 

moisture   i*<* 

organic  matter 148 

sampling 147 

silica    148 

Diffusion  juice   18 

Disc,  Keil,  see  "Keil  disc." 

Disc  pulverizer 170,  178 

Dishes,  moisture   169 

Dorr  thickener 

additional  tests    6u 

discharge   63 

feed    60 

overflow    60 

Draft    75 

Dried  pulp   (see  also  "pulp") 

as   sacked    66 

leaving  dryers   o5 

moisture  in 62,  65,  66,  67 

weekly  analysis  of 66 


INDEX 


255 


Dry  substance   (see  also  "mois- 
ture")     ^.  .  .     2 

by  oven  drying 3 

by  refractometer 3 

in  filter  press  cakes 3,  55,  87 

in  pulp  sold 70 

in  remelt  sugar ^9 

in  uncarbonated  liquors 86 

Drying  ovens 128,  169 

Dust   box    i^3 

Enterprise  meat  chopper.  .170,  178 

Eschka  mixture 129 

Ether,  purification  of 155 

Evaporator  1 1 0 

thick  juice,  see  "thick  juice." 
thin  juice,  see  "thin  juice." 

Excess  water 29 

Extraction,  standard,  tables 

beet    247 

..Steffen 251 

Fat,  see  "crude  fat." 
Feeding   stuffs,   see   "foods   and 
feeding  stuffs." 

Fehling's  solution  18 6 

Fiber,  see  "crude  fiber." 

Filter  cloth  wash  water 30 

Filter  press  cake 

26,  28,  46,  52,  55,  84,  66 

(see    also    "lime   cake,"    "sac- 
charate  cake,"  etc.) 

First  saturation  juice 20 

liquor  82 

Fixed  carbon    129 

Flasks    178,   180 

Flue  gas 

analysis    75 

tables    229,   241,  242j 

temperature    75 

Flume  pulp   20 

Foods  and  feeding  stuffs 151 

ash   156 

crude  fat   155 

crude  fiber    156 

crude  protein   151 

moisture   151 

nitrogen — free  extract  156 

preparation  of  sample 151 


Formulas 

Clerget    G 

hydraulic  presses   176! 

raffinose    6 

Gages,  draft    75 

Gas,  carbonation   85 

flue,  see  "flue  gas." 

lime  kiln   23 

General  methods  1 

Glycerin    170 

Gooch  crucibles  94 

Graduation  marks    181,  185 

Granulated,  available,  tables 

per  cent  on  dry  substance 245 

per  cent  on  sugar 246 

Granulated    sugar,    see    "white 
sugar." 

Graphite   124 

Green    syrup,    see    "high"    and 
"low"  green  syrup. 

Grinding  machinery  170 

Heat  balance    87 

Heat  losses,  calcn.  of 76 

tables 229,  241,  242 

High  green  syrup 32 

High   wash   syrup 32} 

Hilgard   sieve  cylinder 165 

Hot  water  digestion 17,  106 

Humus 16l 

Hydrochloric  acid  190 

(see  also  "muriatic  acid.") 

Hydrometers    171,  182 

Hydrometer  jars   171 

Hydrosulphuric  acid   98,  121 

Hypothetical   combinations    

99,  113,  145 

Ignition  of  precipitates 135 

Indicators  190 

Insecticides    200 

Insoluble    116,   134,  136 

acid    93 

water  93 

Inversion 

hydrochloric   acid   for 190 

sugar  by 4 


256 


INDEX 


Invert  sugar  8 

in   thick  juices 8,  221 

in  thin  juices 9,  222 

Iron 108,  109,  118,  134,  136,  143 

Jar  mill   170,  178 

Keil  disc    ...103,  168,  177 

Kieselguhr,    see    "diatomaceous 

earth." 
Lead  acetate 

basic    190 

dilute   105 

neutral    190 

table 217 

Light   filter    175 

Lime  (see  also  "calcium") 

cake,   first  presses 26 

cake,  second  presses 28 

kiln  gas    23 

milk  of 25,  243 

powder 48 

salts,  see  "CaO  by  soap  soln." 

sewer    28 

to  slacker 25 

Limestone    133 

general 133 

preparation  of  sample 133 

sampling  133 

Limestone  analysis    134,  136 

calcium    134,  137 

calculation  of  results 138 

carbonic  acid    138 

gravimetric  method    134 

insoluble    134,  136 

iron  and  aluminum 134,  136 

magnesium    136 

rapid  method    136 

sulphuric  acid    13ft 

Liquor  entering  factory 82,  86' 

Liter    179 

Lixiviated  ash 10,  93,  107 

Losses,  see  "heat  losses." 

Low  green  syrup 35 

Low  wash  syrup 35 

Magnesia   mixture    112 

Magnesium. .  .109,  118,  136,  138,  143 

Main  sewer  31 

Marking  glassware    181,  185 

Massecuite 31,  34,  35 

alkalinity  of    12 

Meat  chopper 170,  178 


Melted  sugar  (see  also 

"melter"),   44,  45 

Melter,  sugar   36 

Methyl  orange 190 

Methyl  red    190 

Milk    of   lime    25,  243 

Milliliter     179 

Miscellaneous 198 

supplies    200 

Moisture    (see    also    "dry    sub- 
stance")          2 

in  coal  and  coke 128 

in  cotton  seed  cake 158 

in  crude  potash 92 

in  diatomaceous  earth 148 

in  dried  pulp 62,  65,  66,  67 

in  filter  press  cakes 3,  55,  87 

in  foods,  etc 151 

in  remelt  sugar 39 

in    soil 160 

in  sulphur  • 149 

in  white  sugar 32,  198 

Molasses    100 

Baume    101 

bought    100 

in   storage   101 

produced    36,  39 

sold    100 

to  pulp  dryer 62 

worked    39,  47,  80 

Molybdate  solution  112 

Muriatic  acid   199 

Naphthol,    see   "alpha-naphthol." 

Nitric  acid,  standard   195 

Nitrogen,   determination  . . .  .95,  151 

Nitrogen-free  extract 156 

Normal     solutions,     equivalents 

of 244 

Normal  weight 172 

Oil  determination   124 

Organic  coefficient   11 

Organic    matter    145,  148 

Orsat  apparatus   24,  181 

reagents   191 

Ovens,   see  "drying  ovens." 

Oxalic  acid    123 

Oxygen 131 

Pan   storage  tanks    31,  34 

Pebble  mill    170,  178 

Percolation  tests  .  .  33 


INDEX 


257 


Perfectly  washed  cake ...  39,  53,  56 

Phenolphthalein 190 

Phosphoric  acid    112,  121 

Pipettes    180 

automatic    105,  181 

Platinic  chloride  solution 191 

Platinum,  care  of  171 

recovery    191 

Polariscopes     172,  185 

adjustment   of    176 

care  of   176 

cover  glasses    175 

illumination    174 

installation    174 

light    filter    175 

normal  weight   172 

scale    172,  186 

specifications    172 

temperature,  effect  of   173 

tubes     175,  186 

verification    173 

Polarization     3 

tables   218,  220 

temperature,  effect  of  173 

Potash 

bulbs    122 

control    (beet  campaign) 80 

control   (potash  campn.)..82,  141 
crude,  see  "crude  potash." 
determination,  see  "potas- 
sium." 

Potassium,  detn 87,  93,  110,  118 

Potassium  chromate  indicator.  .144 

hydroxide  solution    191 

permanganate     137 

Precipitates,  ignition  of 135 

Presses    176,  178 

Protein,  see  "crude  protein." 
Pulp   (see  also  "dried  pulp"). 

and  pulp  water   19 

and  pulp  water,  flume   20 

dryer  control    62 

entering  presses   64 

entering  silo  69 

flume   20 

leaving  presses    65 

silo  control   69 

sold     69,  228 

water    19,  20 

Pulverizer  ..170,  178 


Purity    6 

apparent    6,  106 

table  of  factors   214 

true    8 

Pyrogallol    191 

Radiator,  Hillebrand    177 

'Raff inose    4,     6 

formula    6 

Rasp    102,  168,  177 

care  of   103 

Raw     massecuite,     see     "remelt 

massecuite." 
Raw  sugar,  see  "remelt  sugar." 

Reagents    188 

Refractometers    3,   177,  186 

Regular  factory  control 16 

Remelt  massecuite 

from  crystallizer  35 

from  pan 34,  39 

Remelt  pan  storage  tanks 34 

Remelt  sugar   35,  39,  44 

Saccharate  cake 

cold    39,  52,  80 

hot   39,  55,  80 

perfectly  washed  39,  53,  56 

Saccharate    milk    39,  56 

Saccharimeters,       see      "polari- 

scopes." 
Sand,    sea    192 

Scales    115 

aluminum    118 

ammonia    123 

calcium    118 

carbon    124 

carbonic  acid    121 

chlorine    119 

copper    116 

graphite    124 

hydrosulphuric  acid   121 

insoluble     116 

iron    118 

magnesium    118 

oil     124 

oxalic   acid    123 

phosphoric  acid   121 

potassium    118 

preparation   of  sample    115 

qualitative  examination    115 

quantitative  examination   116 

sampling    115 


258 


INDEX 


silica    116 

sodium    118 

sugar   124 

sulphuric   acid    119 

sulphurous  acid   120 

zinc 118 

Screen  tests  49,  97 

Sea  sand    192 

Second    saturation   juice 21,  42 

Sewer 

lime 28 

main    31 

Sieve  cylinder   165 

Sieve    tests    .49,  97 

Silica    107,  116,  142,  148 

Silver  nitrate  solution 144 

Slacking  test    49 

Soap  solution 

CaO  by 13 

standard 196 

tables    224,  226 

Soda  ash   199 

caustic    199 

Sodium    110,  118 

ammonium  phosphate   193 

carbonate    192,  193 

(see  also  "soda  ash") 

chloride    144 

hydroxide,  standard   195 

oxalate    137 

phosphate    193 

thiosulphate    117 

Soil    160 

preparation  of  sample 160 

sampling    160 

Soil  analysis  160 

carbon    dioxide 161 

humus    161 

inorganic  constituents   161 

mechanical    analysis    162 

moisture    160 

nitrogen,  total    160 

statement  of  analysis   166 

volatile   matter    160 

water  capacity  165 

water    soluble    161 

Solids,   total    142 

Solution  for  cooler  .  .   47 


Specific  gravity  tables 

of  sugar  solutions 201 

of  various  materials  251 

Speeds  of  lab.  machinery 177 

Standard  acid  and  alkali  193 

Standardization  of  apparatus . . .  179 

bibliography .186 

Starch  indicator    117 

Steam  calculation  87 

Steffen  process  control  47 

Storage  tanks    31,   34,  101 

Sugar    (see    also    "white"    and 
"remelt"  sugar) 

by  cold  water  digestion   105 

by  direct  polarization 4 

by  hot  water  digestion  ...  17,  106 

by    inversion    4 

detection  by  alpha-naphthol . . 

14,    37 

in   scales    124 

Sugar  melter    36 

Sugar-soluble  CaO    49 

Sulphate  cake    46 

Sulphate  control   42 

Sulphated   ash    9 

Sulphates,  see  "sulphuric  acid." 
Sulphides,    see    "hydrosulphuric 

acid." 
Sulphites,  see  "sulphurous  acid." 

Sulphur     149 

in  coal    129 

sampling    149 

Sulphur  analysis   149 

arsenic    150 

ash: 149 

moisture     149 

sulphur     149 

Sulphuric  acid 
detn.   ...11,  98,  112,  119,  136,  144 

standard     194 

Sulphurous   acid    120 

Suspended   matter    145 

Sweet    water    30 

Tables     201 

(see   table   of   contents    for 
list) 

Tailings,    see   "beet   tailings." 
Temperature  correction  tables 

for  Abbe  refractometer    216 

for    Brix    hydrometers. .  .215,  216 


INDEX 


259 


Temperature  data    ...40,  §9,  67,  8G 

Thermometers     178,  185 

Thick  juice 

blow-up 23,  43 

evaporator    22,  39 

Thick  liquor   83,  85,  86 

Thin  juice,  evaporator 22 

Thin    liquor    83,  86 

Third  saturation  juice   21,  43 

Total  solids  142 

Total  sulphates    142 

True   purity    8 

Undetermined     40 

Vacuum  pump    178 

Volatile   matter    128 

Volumetric  apparatus   178,  179 

Wash    syrup,    see    "high"    and 

"low"  wash  syrup. 
Wash  water 

cold    51 

hot    52 

Waste  water 

cold  press    50 

cooler    49 

hot   filter    61 

total    50,  81 

Water    139 

bacteriological    examination  .  .139 

battery  supply   141 

boiler    38,  84 

condensed     37,  84 

distilled    197 

from    presses    63 


from  pulpefanger    63 

quality  of   7,  197 

sampling    139,  140 

Water   analysis    141 

calcium     143 

carbonic  acid    145 

chlorine    143 

example    145 

hypothetical    combinations    . .  145 

iron    143 

magnesium     143 

organic  and  volatile  matter..  145 

silica    142 

statement  of  analysis    146 

sulphuric   acid    144 

suspended  matter   145 

total  solids    142 

total    sulphates    142 

Water  capacity    165 

Water    insoluble    93 

Water   soluble    161 

Weekly  analysis  of  dried  pulp . .   66 

Weekly  composite  samples 

38,   80,  86,  141 

Weights    185 

White   massecuite    31,  39 

White  pan  storage  tanks  31 

White  sugar 

moisture  in    32,  198 

percolation  tests  of   33 

sampling    of    198 

sulphuric  acid  in 44 

Zinc,  determination    118 

Zinc  nitrate  solution   .  . .  197 


YC  704(8 


468640 

'^S'^ 


UNIVERSITY  OF  CALIFORNIA  LIBRARY 


